The Forever‑Changing World of PFAS Testing

The forever changing world of PFAS testing The PFAS eBook from SCIEX2 | sciex.com 3 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle The PFAS lifecycle: an overview Craig M. Butt SCIEX Jianru Stahl-Zeng SCIEX These MCLs cover PFOA and PFOS (4 ng/L or parts-per-trillion), and PFHxS, PFNA and HFPO-DA (10 ng/L). PFBS is also covered by a hazard index approach in samples containing PFAS mixtures. The final rule also requires all public water systems to complete initial monitoring by 2027 and, if exceedances are found, to implement reduction solutions by 2029. In addition, several states have established their MCLs or guidance levels for PFAS in drinking water. How do these drinking water regulations in the United States impact the PFAS lifecycle? In 2021, the US EPA established its PFAS Strategic Roadmap, which ran until 2024. A guiding principle of this roadmap was the PFAS lifecycle and understanding the source of PFAS contamination by driving to the root cause. As a result, EPA 1633A was finalized for the analysis of PFAS in wastewater, surface water, groundwater, soil biosolids, sediment, landfill leachate, and fish tissue. These matrices are more complex and inherently challenging, placing increasing demand on instrument performance. In January 2021, the European Union began enforcing PFAS drinking water levels as part of their Drinking Water Directive. The limits are 100 ng/L for the sum of 20 PFAS compounds and 500 ug/L for “total PFAS”. In October 2022, the European Commission proposed a standard for surface and groundwater for 24 PFAS compounds at 4.4 ng/L (as PFOA equivalents). The lower limits will require lower reporting limits and presumably novel analytical methods to meet these limits. Consumer products have also been subject to recent or proposed regulations in the United States and European Union. A wide PFAS ban has been proposed in the European Union, although the details have not been finalized. In February 2025, France approved banning the manufacture, import and export of PFAS-containing consumer products, including cosmetics, textiles and footwear. Similar bans have been passed in several US states, including New York and California. Some regulations also cover food packaging. Personal care products, such as cosmetics, may accumulate in the body during dermal absorption, or enter the wastewater systems after wash-off. Similarly, textiles may contribute to wastewater PFAS regulations continue to accelerate around the globe. Recent years have seen regulations evolve beyond drinking water and include other matrices in the PFAS lifecycle such as food and consumer products. contamination and may be a source to landfills during disposal. In addition, the PFAS used in our consumer products may end up in our house dust, which can be ingested by humans and our pets. The need to protect human health and the environment has necessitated a full understanding of the PFAS lifecycle. As such, regulations on so-called “upstream” matrices such wastewater, surface waters and consumer products are expanding. Researchers will need to adapt our current methods to study these novel matrices, presumably with lower and lower detection limits. Innovation in our mass spectrometry will be crucial to meet these demands. Contents 01 The PFAS lifecycle an overview 02 PFAS the global headline maker regulations from around the world 03 Industry collaborations a customer success story 04 Addressing the challenges of PFAS testing 05 Solutions at every level 06 SCIEX OS when software compliments hardware 07 PFAS around the world regional trends 08 After-sales, service, and support for all your needs 09 On-demand customer collaborations 10 Technical materials for each component of the PFAS lifecycle 11 Phenomenex your partner in PFAS-testing consumables The PFAS lifecycle: an overview4 | sciex.com 5 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle PFAS – A global headline maker Every day, it seems like there’s a new headline about Per- and polyfluoroalkyl substances (PFAS) restrictions being implemented somewhere. Stories like “Forever Chemical used on Jersey’s Potato crops” or “Are PFAS in everything? What you need to know about ‘forever chemicals’” grab attention and raise concerns globally. After all, most of us consume food and water or use products that might have been exposed to PFAS at some point. PFAS isn’t a new issue; it dates back to the 1940s when it revolutionized non-stick, heat-resistant products. From household items like furniture, wall paint, and carpets to industrial uses like electrical wire coatings, firefighting foams, and cosmetics, PFAS has been widely adopted. However, unlike its initial promise, this chemical group leaves a lasting impact on the human body and the environment. Numerous studies have highlighted the toxicity of PFAS, classifying it as carcinogenic and an endocrine disruptor. The dangers of PFAS are welldocumented, prompting regulators across various industries to impose strict testing and reporting procedures. These measures ensure water quality is safe and PFAS levels are within acceptable limits. Guidelines are also issued for PFAS levels in the food chain, and policies are being developed for manufactured products and personal care items like clothing and makeup. A significant regulatory move came in 2022 when the US Environmental Protection Agency (EPA) issued drinking water health advisory levels (HALs) for four PFAS compounds. In response, companies like SCIEX, Eurofins, and Phenomenex developed detailed methods to detect these compounds at extremely low levels. This advisory underscores the seriousness with which regulators are addressing PFAS contamination. Regulatory efforts aren’t limited to the United States. Around the world, national standard agencies have been rigorously governing PFAS in drinking water, raw waters, and wastewaters for years. Their focus has now expanded to include food, produce, and manufacturing processes. The following map highlights some of the regulations being implemented globally to manage and control PFAS in various regions. companies are exploring new materials and technologies that can provide the same benefits without the harmful environmental and health impacts. Public pressure and advocacy are also playing a crucial role in pushing for stricter regulations and more transparency from manufacturers. In the meantime, individuals can take steps to reduce their exposure to PFAS by being mindful of the products they use and the food they consume. Opting for PFAS-free products, filtering drinking water, and staying informed about local An insight into the various bodies around the world driving policy, guidelines and regulation. regulations and advisories can help US EPA regulations EU water framework directive mitigate the risks associated with these persistent chemicals. The collective effort of regulators, industries, and consumers will be essential in moving towards a PFAS-free future. EPA 537 (Micro LC + 6500+): Analysis for PFAS using microflow liquid chromatography EPA 537.1 (4500): Analysis of PFAS in drinking water EPA 537 (5500): Quantitation of PFAS in water samples using LCMS large-volume injection and solid phase extraction EPA 533 (4500): Analysis of PFAS at low ppt levels in drinking water An ultra-high sensitivity analysis of PFAS compounds in multiple water sources Quantitation of PFAS in food with parts per trillion levels of sensitivity EPA 533 (5500+): PFAS analysis in drinking water at low parts-per-trillion levels p 1 Analysis of PFAS at low ppt levels in drinking water via EPA method 533 Using the SCIEX Triple Quad 4500 system Matthew Standland, Craig M. Butt, and Matthew Noestheden SCIEX, USA Per- and polyfluorinated alkyl substances (PFAS) are a group of manmade chemicals that have been used for decades in a large host of applications. A recent review focused on 1,400 unique PFAS species1 although current OECD databases have upwards of 4,500 unique PFAS compounds.2 The resilience of some PFAS to degradation and their potential for biological harm have spurred health and environmental concerns amongst regulatory agencies. The CDC’s national biomonitoring program has found evidence of widespread presence of certain PFAS residues in human serum3. One possible route of human exposure is from PFAS contaminated water.4 PFAS are known to enter the water supply and bioaccumulate in watershed ecosystems. This can be a health issue for humans who directly consume contaminated water. The US EPA published the fifth unregulated contaminant monitoring rule (UCMR5)5, which proposes maximum residue limits (MRL) for PFAS residues in EPA method 533. Representative chemical structures are shown in Figure 1. This technical note presents data collected in accordance with EPA method 533 requirements for the initial demonstration of capability (IDC). Sample preparation was done using Phenomenex Strata-X-AW Weak Anion solid-phase extraction (SPE) and data acquisition was performed using the SCIEX Triple Quad 4500 system coupled to an ExionLC AC system. Key method features • MRLs ≤ 3 ng/L reported for all analytes, meeting UCMR5 requirements for EPA method 533 compounds • Sensitive and robust performance meets all EPA method 533 performance criteria • SCIEX OS software simplifies data review and report generation using custom calculations and flagging rules • Specialized LC setup ensures low systemic contamination Figure 1. Representative structural diversity among EPA method 533 analytes. Compounds can have either sulfonate (left) or carboxylate head groups (right). Structure variability can also include per-/polyfluorinated species, the presence or absence of ether linkage(s) and alkyl chain length with or without branching. p 1 For research use only. Not for use in diagnostics procedures. Confidential - Company Proprietary An ultra-high sensitivity analysis of PFAS compounds in multiple water sources Using the SCIEX 7500 System Bertram Nieland1, Jack Steed2, Rens-Jan Jaspers3, Kay Hup3, Abdessamad Chahbouni3, Jianru Stahl-Zeng4 1SCIEX, The Netherlands; 2SCIEX, UK; 3Het Waterlaboratorium, 4SCIEX, Germany In this method sub-parts per trillion (ppt) levels of detection for 26 PFAS compounds was achieved with LOD values of 0.2 ng/L in diluent and calculated method detection limits in drinking, ground, and surface water ranging between 0.06 ng/L and 1.12 ng/L. PFAS compounds are ubiquitous in our environment due to overuse and their lack of breakdown, ensuring that this will be a challenge for decades to come.1 Therefore, it is imperative to provide rigorous and sensitive analytical testing to regulate these compounds and try to limit their possible effects on human health. In December 2020, the European Parliament and Council of the European Union released a new directive that sets the limit of PFAS in drinking water to 0.5 µg/L for all PFAS compounds identified, and 0.1 µg/L for a subset of PFAS compounds that are particularly concerning for humans. The difference between the limits is dependent on a list of compounds stated within the directive. The 0.1 µg/L limit applies to the compounds included in this list, which contain a perfluoroalkyl moiety with 3 or more carbons (i.e., –CnF2n–, n ≥ 3) or a perfluoroalkylether moiety with 2 or more carbons (i.e., –CnF2nOCmF2m−, n and m ≥ 1). The 0.5 µg/L limit applies to all PFAS compounds in total 2 This method is suitable for drinking water, surface water and groundwater. Testing of surface and ground water is important to ensure that these water sources are not contaminated and that drinking water sources are not affected. Key features of PFAS analysis using the SCIEX 7500 System • Ultra-high levels of sensitivity with LOQ values between 0.2 ng/L and 2.0 ng/L. See Figures 1 and 2 which highlight the sensitivity achieved. • Calculated method detection limits between 0.06 ng/L and 1.12 ng/L in three different water matrices • Twenty-six relevant PFAS compounds analyzed in LC-MS grade, drinking, ground and surface water • The mitigation of equipment which can cause PFAS contamination to decrease blank contamination and interference at the analyte retention time Figure 1. Extracted ion chromatograms (XICs) of three PFAS compounds at their respective LOQs. From left to right: PFBS, PFHxA and PFOS – all at 0.2 ng/L. The image above shows excellent sensitivity has been achieved with this method at low ng/L levels. PFBS PFHxA PFOS Xanthippe Theurillat1, Claudia Mujahid1, Bjorn Eriksen1, Ashley Griffin2, Andrew Savage2, Thierry Delatour1, Pascal Mottier1, Jack Steed3, Michael Scherer4, Jianru Stahl-Zeng5 1Société des Produits Nestlé, Nestlé Research; 2Société des Produits Nestlé, Nestlé Quality Assurance Center, 3SCIEX, UK; 4SCIEX, Switzerland; 5SCIEX, Germany This technical note demonstrates a validated method for the analysis of 57 per- and polyfluoroalkyl substances (PFAS) compounds in a diverse range of food matrices. Using the SCIEX 7500 system and a simplified extrac�on method, the limit of quan�ta�on (LOQ) levels met the Commission Regula�on EU 2022/2388 for the 4 regulated PFAS compounds, including: PFOS, PFOA, PFNA and PFHxS. Specifically, LOQs were as low as 0.01 µg/kg for some PFAS in the food matrices (Table 1).1 The low LOQ levels were due to the sensi�vity of the SCIEX 7500 system and the extensive contamina�on reduc�on steps that were implemented to reduce the PFAS background signal. The 7 food matrices tested included, baby food puree (beef), milk-based infant formula (as sold), full cream milk powder, fish, whole egg, soluble coffee and fish oil. The method showed good precision at the LOQ level for the 4 regulated compounds. The %CV was <20% for most matrices and <25% for all matrices. For more informa�on refer to the publica�on on which this technical note is based.2 Key features of PFAS analysis in multiple foods when using the SCIEX 7500 system • Broad PFAS coverage. A method was developed and validated for 57 PFAS compounds following the EURL POPs guidelines. • Diverse food matrices. Mul�ple food matrices were tested including baby food puree (beef), milk-based infant formula (as sold), full cream milk powder, fish, whole egg, soluble coffee and fish oil. • Parts-per-trillion (ppt, µg/kg) sensi�vity. LOQs in food matrices analysed were as low as 0.01 µg/kg Quan�ta�on of PFAS in food with parts per trillion levels of sensi�vity Table 1. The EU recommended (Rec.) and achieved LOQ in-sample concentra�ons for the 4 regulated PFAS compounds. All units are in µg/kg. (For more details, please see Tables 2 to 5). a: LOQ; b: indica�ve level. Indica�ve levels specify that further inves�ga�on needs to be performed however, this does not stop the products from being put on the market. Matrix PFOS PFOA PFNA PFHxS Rec. Achieved Rec. Achieved Rec. Achieved Rec. Achieved Eggs 0.3a 0.3 0.3a 0.3 0.3a 0.3 0.3a 0.3 Fish 0.1a 0.1 0.1a 0.1 0.1a 0.1 0.1a 0.1 Food for infants and young children 0.05b 0.01 0.05b 0.01 0.05b 0.01 0.05b 0.01 p 1 EPA method 533 for PFAS analysis in drinking water at low parts-per-trillion levels Using the SCIEX Triple Quad™ 5500+ LC-MS/MS System – QTRAP® Ready Craig M. Butt1, Karl A. Oetjen1, Thep Phomsopha2 1 SCIEX, USA; 2 Eurofins ETA West Sacramento, USA This application note describes PFAS drinking water analysis by EPA Method 5331 using the SCIEX Triple Quad 5500+ LCMS/MS System – QTRAP Ready. Excellent sensitivity and precision were shown. The “in-sample” minimum reporting limits were 2 ng/L for all analytes except PFHpA (4 ng/L). Figure 1 shows MRM chromatograms for the novel perfluorinated ether carboxylic and sulfonic acids in the 0.50 ng/mL standard, which corresponds to 2 ng/L in sample. These values are significantly below the US EPA drinking water guidelines of 70 ng/L for PFOS and PFOA. Use of the custom built calculations and flagging rules within the SCIEX OS Software were used to streamline data review and report generation. EPA Method 533 builds upon the previously published EPA Methods 537 and 537.1, but with notable differences. Several odd-chain PFSAs, short-chain PFCAs, FTS compounds and novel perfluoroether carboxylates and sulfonates were added, whereas the FOSAA acids (NEtFOSAA, NMeFOSAA) and longchain PFCAs (PFTA, PFTrDA) were excluded. Structures of the novel compounds are shown in Figure 2. Similar to previous EPA methods, water samples are concentrated using solid-phase extraction (SPE) cartridges, but the choice of cartridge is flexible and the sample volume can vary from 100-250 mL. In addition, Method 533 incorporates the use of stable isotope dilution standards to minimize matrix effects and improve data quality. Key features of EPA method 533 on the SCIEX 5500+ System • Existing methods were adapted to meet challenges of novel PFAS compounds • Minimum reporting limits of 2 ng/L with excellent linear dynamic range were achieved • Method showed good peak and chromatographic resolution of all compounds • Data review and report generation was simplified through use of SCIEX OS Software custom calculations and flagging rules Figure 1. MRM chromatograms for novel perfluorinated ether acids. MRM XICs for the novel perfluorinated ether acids are shown from the 0.50 ng/mL in-vial standard (2 ng/L in sample equivalent). p 1 EPA method 533 for PFAS analysis in drinking water at low parts-per-trillion levels Using the SCIEX Triple Quad™ 5500+ LC-MS/MS System – QTRAP® Ready Craig M. Butt1, Karl A. Oetjen1, Thep Phomsopha2 1 SCIEX, USA; 2 Eurofins ETA West Sacramento, USA This application note describes PFAS drinking water analysis by EPA Method 5331 using the SCIEX Triple Quad 5500+ LCMS/MS System – QTRAP Ready. Excellent sensitivity and precision were shown. The “in-sample” minimum reporting limits were 2 ng/L for all analytes except PFHpA (4 ng/L). Figure 1 shows MRM chromatograms for the novel perfluorinated ether carboxylic and sulfonic acids in the 0.50 ng/mL standard, which corresponds to 2 ng/L in sample. These values are significantly below the US EPA drinking water guidelines of 70 ng/L for PFOS and PFOA. Use of the custom built calculations and flagging rules within the SCIEX OS Software were used to streamline data review and report generation. EPA Method 533 builds upon the previously published EPA Methods 537 and 537.1, but with notable differences. Several odd-chain PFSAs, short-chain PFCAs, FTS compounds and novel perfluoroether carboxylates and sulfonates were added, whereas the FOSAA acids (NEtFOSAA, NMeFOSAA) and longchain PFCAs (PFTA, PFTrDA) were excluded. Structures of the novel compounds are shown in Figure 2. Similar to previous EPA methods, water samples are concentrated using solid-phase extraction (SPE) cartridges, but the choice of cartridge is flexible and the sample volume can vary from 100-250 mL. In addition, Method 533 incorporates the use of stable isotope dilution standards to minimize matrix effects and improve data quality. Key features of EPA method 533 on the SCIEX 5500+ System • Existing methods were adapted to meet challenges of novel PFAS compounds • Minimum reporting limits of 2 ng/L with excellent linear dynamic range were achieved • Method showed good peak and chromatographic resolution of all compounds • Data review and report generation was simplified through use of SCIEX OS Software custom calculations and flagging rules Figure 1. MRM chromatograms for novel perfluorinated ether acids. MRM XICs for the novel perfluorinated ether acids are shown from the 0.50 ng/mL in-vial standard (2 ng/L in sample equivalent). p 1 Analysis of PFAS in drinking water with EPA method 537.1 and the SCIEX QTRAP 4500 system Achieving 537.1 method requirements in a robust 10-minute method Simon Roberts1, Craig Butt1, Dan Wright2, Stephen Somerville2, KC Hyland1, Chris Borton1 SCIEX, USA1, EQI, Columbia, SC, USA2 In the United States, EPA method 537.1 describes the sample preparation, reporting guidelines, and quality control for the analysis of a suite of 14 per- and polyfluorinated substances (PFAS) in drinking water. The EPA 537.1 method guidelines provide some flexibility in the liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis. Within these guidelines, optimization of certain aspects of the method, such as column chemistry, chromatography, mobile phases, gradient profile, and MS/MS transitions, was performed. Sample preservation and preparation guidelines published in EPA 537.1 are prescriptive and were therefore closely followed. Key features of PFAS analysis on the SCIEX QTRAP 4500 system • Robust and reproducible results with qualifying accuracy and precision for calculated concentrations, asymmetry factor, and linearity • Total sample runtime takes only 8-10 min, depending on autosampler settings and system dead volume • Sensitive MDLs of 0.08-0.2 ng/L for the entire suite of 14 PFAS compounds Table 1. PFAS in EPA method 537.1. Names, abbreviations, and method detection limits (MDLs) for 14 PFAS compounds included in EPA Method 537.1 along with the reporting limits (MRLs) published by the UCMR3 guidelines 6 of the PFAS compounds. MDLs and MRLs shown as ng/L (ppt) here. Compound Abbreviation Method detection limit (ng/L) UCRM3 reporting limit (ng/L) Perfluorohexane carboxylate PFHxA 0.09 - Perfluoroheptane carboxylate PFHpA 0.1 10 Perfluorooctane carboxylate PFOA 0.1 20 Perfluorononane carboxylate PFNA 0.09 20 Perfluorodecane carboxylate PFDA 0.1 - Perfluoroundecane carboxylate PFUnDA 0.1 - Perfluorododecane carboxylate PFDoA 0.1 - Perfluorotridecane carboxylate PFTrDA 0.2 - Perfluorotetradecane carboxylate PFTeDA 0.2 - Perfluorobutane sulfonate PFBS 0.1 90 Perfluorohexane sulfonate PFHxS 0.08 30 Perfluorooctane sulfonate PFOS 0.1 40 n-ethyl perfluorooctane sulfonamidoacetic acid n-EtFOSAA 0.1 - n-methyl perfluorooctane sulfonamidoacetic acid n-MeFOSAA 0.09 - p 1 Quantitation of PFASs in water samples using LC-MS/MS large-volume direct injection and solid phase extraction Simon Roberts1, KC Hyland1, Craig Butt1, Scott Krepich2, Eric Redman3, and Christopher Borton1 1SCIEX, USA; 2Phenomenex, USA; 3TestAmerica Laboratories, Sacramento, USA PFASs are unique chemicals whose physicochemical properties make them important for use in a variety of industrial and consumer products including carpets, cookware, food packaging, fire suppressants, and others1. Chemically, PFASs are aliphatic structures containing one or more C atoms on which H substituents have been replaced by F atoms. Classification and naming is typically by the particular functional group present, such as carboxylic acids, sulfonates, phosphonic acids, etc., as well as the length of the carbon chain. Desirable in various industrial applications for their chemical stability and low reactivity, these properties also make PFASs highly resistant to degradation in aquatic environments. Typical concentrations of PFASs found in various environmental water sources range from pg/L to µg/L levels2. Human exposure to PFAS residues has been implicated in the incidence of cancer, obesity, endocrine system disruption, and other adverse health effects3-4. In recognition of these potential risks, sources of human exposure to these chemicals (e.g., via drinking water) are receiving public and scientific attention. PFASs exhibit relatively high aqueous solubility and can be transported and bioaccumulated from contaminated water sources. The US EPA maintains health advisory limits for select PFASs (e.g., perfluorooctanoic acid (PFOA) at a limit of 70 ng/L) in water, but these levels have been exceeded in some areas experiencing extreme point source inputs of these chemicals5. Given the tremendous persistence of PFASs in the environment and their known presence in human populations exposed via drinking water and other environmental routes, demonstration of the capability for accurate and precise low-level quantitation is paramount for research and testing laboratories. Robust quantitative analytical methods utilize the specificity and sensitivity of LC-MS/MS with MRM monitoring. However, a primary analytical challenge to this assay is the prevention and reduction of background PFASs originating from the LC system and contamination during sample collection and preparation. This application note presents two methods for the quantitation of per- and polyfluorinated alkyl substances (PFASs) in water samples. While the MS/MS detection method using the SCIEX Triple Quad™ 5500 System is similar between the two methods, the sample preparation and injection volume differ significantly. Key features of PFAS methods • LC-MS detection using a Shimadzu LC-20ADXR coupled to a SCIEX Triple Quad™ 5500 System • Special modifications to the pumps and autosampler are described to mitigate laboratory-based contamination of PFASs. • Use of a delay column for separation of a contamination PFAS peak from the analytical peak • The first method presented here utilizes a weak-anion exchange solid phase extraction (SPE) method to concentrate water samples for analysis using a 7.5 minute HPLC gradient. • The second method utilizes dilution of a water sample in methanol and direct injection of 950 µL of the diluted sample using a 17.5 minute HPLC gradient. • Large volume injection of an aqueous sample is intended to achieve method sensitivity while reducing accumulated background during sample concentration steps. • Both methods achieved accurate quantitation at levels of approximately 1-10 ng/L for more than 17 PFASs. The PFAS lifecycle: an overview6 | sciex.com 7 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle PFAS regulations around the world Canada Driving down from 30ng/L to 25ng/L A goal of 30 ng/L for 25 PFAS in drinking water to reduce health risks. This replaces previous guidelines for PFOS, PFOA, and nine other PFAS. The target is precautionary and based on achievable treatment methods. United States First ever nationwide drinking water standards The EPA’s new regulation limits six PFAS chemicals in drinking water, aiming to protect 100 million people and reduce health risks, with $1 billion in funding to support compliance. Brazil Brazil’s Strides Towards Regulating PFAS: Uncovering New Regulatory Initiatives Brazil’s National PFAS Control Policy Bill No. 2726/2023 aims to regulate PFAS by enforcing environmental preservation, requiring annual reports from companies, and promoting public awareness and research. The bill has passed the first approval stage and will move to the senate if it clears all stages. Argentina Lowest PFAS levels in the world This study is the first to track human PFAS exposure in Argentina, finding the lowest maternal PFAS levels globally. South Africa Production and distribution prohibition South Africa regulates per- and polyfluoroalkyl substances (PFAS) by prohibiting the production, distribution, and import of certain PFAS. These regulations took effect in December 2021. Australia Lower limits proposed for drinking water Australian Governments are managing PFAS contamination by investigating its extent, breaking exposure pathways, supporting communities, funding research, reviewing legislation, and improving coordination across government levels. China Chinese government is working to - reduce PFAS discharge from industrial sources. China’s Miniatry of Ecology and Environment has drafted a pian to Inanage new poliutants. The plan includes strict ragulationa on new chamicalrepstrations, bans on harntul chemicala, and morous standards for hazardous chemica, content products. Japan Ban on 138 Chemicals The Japanese government proposed banning 138 PFAS chemicals on January 10, 2025. The ban will prohibit the manufacture, import, and use of these chemicals. France PFAS ban passed France has passed a new law banning PFAS (per- and polyfluorcalky! substances) in products like clothing and cosmetics. PFAS are known as “forever chemicals” due to their persistence in the environment and links to health issues such as cancer and reduced fertility. Despite some opposition and the exclusion of cookware from the ban, this law is a significant step towards protecting public health and the environment. United Kingdom A precautionary approach to regulation In August 2024, the DWi updated guidelines for PFAS in drinking water. Water companies in England and Wales must monitor more PFAS and update risk assessments. The limit is 0.1 micrograms per litro for 48 specified. PFAS the global headline maker: regulations from around the world8 | sciex.com 9 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Industry collaborations 0310 | sciex.com 11 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Industry collaborations: a customer success story S: Can you tell us a little bit about OCWD? LS: Here at Orange County Water District, we have over 225 employees and our lab consists of 35 team members including five to six student interns. I’ve worked here over 30 years, so having spent more than half of my life here, I look at OCWD as my second home! Our main goal is to follow and adhere to EPA standard methods for monitoring drinking water quality, groundwater surface water, and recycled water. We conduct routine analysis on a daily basis for results reporting. We test approximately 1500 locations throughout the central and northern Orange County, including about 200 drinking wells, while serving over 2.5 million residents. S: What do your day-to-day responsibilities look like? LS: I stand as the working supervisor, and I love being hands-on with the method development process. When a new PFAS testing method surfaces, I am the one who sets up and develops the method. On completion, the method is certified online, then my responsibility shifts to training our staff. I and another co-supervisor oversee the daily operation of our lab. Our instrument portfolio includes GC, GCMS, LC, HPLC, LC-MS/MS, and each team member is responsible for certain methods. For methods like 524.2, we would have a team of three staff members on samples as it’s a heavy workload compared to other automated methods. Every morning, we have a group meeting: So what needs to be done? Who’s doing what? Each analyst would decide who is processing and running which sets of samples, and be prepared for any reruns, retracts, or resampling. Once complete, then the process moves to date analysis and reporting. Sometimes, it can be 1-2 hours a day as my job also includes trouble shooting and problem solving! Even though it’s a workplace, it’s always like a big family with everyone. I try to make as a better place, and I always enjoy being here every day. S: Many of our users want to know how you tackle the common problems other labs face: contamination, sample prep, the usuals! LS: We are very good as a lab to handle, and control, PFAS background. If we had a background problem, we would troubleshoot and determine if it’s coming from the extraction, or from the instrument, or from sample collection. Step 1 – if the sample blank passes, then that confirms the instrument is fine and we eliminate that potential and re-evaluate the extraction process. Is it the filtration plate? Are there other potential sources? Our protocol ensures this is a rare occurrence though. S: How do you ensure data quality? Do you participate in any Proficiency Testing programs? LS: We perform PT every year between April and May, when we do PT for both 533 and 537 and all other methods within our lab. Our staff is great for this because we always get 100%! S: What has been your biggest challenge and how did you overcome that? LS: That has to be when I first started setting up methods back in 2011, when there were not too many people testing for PFAS at the time. I had to figure out myself. Background contamination was the biggest challenge, for PFOA, as well as LC separation. This is where the community, and SCIEX, helped by suggesting tweaks like delay columns. Carryover was also a concern, but eventually solved by automation. So my advice for anyone out there is to connect with your community and vendor. S: We are always here to help and provide an educational platform for all interested users. How do you think is the best way for us to deliver this? LS:For me, it is technical support and application notes: if the person have never done the method or have no experience with LCMS, I think it would be good for a vendor to provide the application note, guide them through the process, and develop the method with them. So I think the best way is help the customer with PFAS testing, is start with the basic method, and they can improve from there. For us internally, the most important thing the analyst needs to learn is: how to troubleshoot a problem. This is to minimize downtime. We go through data review regularly to make sure that they know what to look for, like PFAS peaks. I personally set out two or three solid days with each analyst, to make sure they understand everything, and go through initial demonstration capability. They have to demonstrate the capability of three-day MDL and calculate the PIR. We have very extensive training: What does good look like? A sneak-peek into Orange County Water District. We had the privilege of interviewing Dr Lily Sanchez, Supervising Chemist at OCWD, a collaborating lab, to gain an insight of how an industry leading water testing facility is run to the highest standards. SCIEX (S), Dr Lily Sanchez (LS) SCIEX provides us with a lot of support. SCIEX is always my number 1 go-to, so it is the combination of community collaboration and vendor contacts. We analyze PFAS daily, with two 6500s, running up to 120 samples across both Even though it’s a systems routinely. workplace, it’s always like a big family with everyone. I try to make it a better place and I always enjoy being here every day. Dr Lily Sanchez Supervising Chemist at Orange County Water District (OCWD) Industry collaborations: a customer success story12 | sciex.com 13 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle checklists of what needs to be done at each stage, and once they pass all of that, only then can they can report the data. They are then considered qualified analysts for date reporting for the method they are assigned, as PFAS testing is a constant training course! S: What about the future? What do you see if the next trend in testing for PFAS in drinking water? LS:From what I’m seeing lately, it’ll be direct injection methods. I’m on the standard method committee, and we’re trying to develop that too. So for the future, I think that we’ll need more sensitive and faster methods, which means more advanced LCMS instruments. I want a 7500 for our lab! So direct injections will be more common. Reduced time means money saving and shorter turnaround times: results within 1 hour is ideal. Attention is also shifting to non-targeted analysis, and total organic fluorene. I expect to see more compounds required on the regulatory list, groundwater analysis, and additional responsibilities for government agencies like us to clean up those wells. So for PFAS testing, it will depend on how we adapt, develop methods to be faster and more reliable, so we can meet those growing PFAS demands. S: As we close this insightful interview, anything you’d like to add? LS: The SCIEX and Phenomenex staff that I’ve worked with, I feel like I can always go ask them whenever I have questions or problems. I come to them and they’re always a good resource for me. They’re always helping me, whenever I have a This technical note demonstrates the use of the PromoChrom automated solid-phase extraction (SPE) system for the analysis of PFAS in drinking water following EPA Method 533. Using the SCIEX QTRAP 6500+ system, negligible background contamination was observed as well as excellent method performance in spikes into reagent water and raw untreated groundwater samples. Milli-Q water blank spikes at 2, 40 and 70 ng/L showed mean recovery ranging from 96% to 115% with the mean precision <10% coefficient of variation (CV). Sample matrix and duplicate spikes at 2 and 40 ng/L showed mean recovery between 95% and 122% with <13%CV. Analysis of raw untreated groundwater samples showed the detection of 5 out of the 6 EPA-regulated PFAS compounds. Industry collaborations: a customer success story Automated solid-phase extraction system for the analysis of PFAS in drinking water problem, they provide suggestions, and t’s always worked out. And if not, they will send me to somebody else. So I really appreciate all of that. The support. S: Well that is great to hear, and our internal PFAS is always happy to help any way we can. Thank you Lily, for providing us your perspective into your world of PFAS testing! To learn more about what Orange County Water County does, check out this video: Industry collaborations: a customer success story14 | sciex.com 15 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Industry insights In the dynamic field of water testing, laboratories are facing an everincreasing sample load. More than ever, the robustness of testing systems has become a crucial factor in delivering reliable results. Hup and Abdessamad Chahbouni from HET Waterlaboratorium in The Netherlands, in collaboration with the SCIEX European support team and Jianru Stahl-Zeng, have developed a method that stands out for its robustness. This refined method is now running as a routine application with unmatched reliability, becoming a significant asset to their laboratory’s offerings. At HET Waterlaboratorium, 26 PFAS compounds of interest can be measured in diverse water samples, ranging from drinking water to ground and surface water. This broad and reliable offering sets the lab apart in the industry. In 2020 the European Dring Water Directive set the limit of PFAS in drinking water to 0.5 µg/L for all identified PFAS compounds. To ensure the safety of drinking water the analysis of ground water sources for contamination is vital to protect drinking water sources. The robustness of the method developed by HET Waterlaboratorium is demonstrated over a 15-month period, during which preventive maintenance was required only once. Prior to this maintenance, calibration specifications were consistently met with only front-end cleaning needed. This level of robustness is unmatched in the industry, providing confidence and reliability in the testing process. The labs work includes collaborations with Japanese research institutions and involvement in PFAS-related research beyond laboratory analysis, such as tracking PFAS trends and exploring PFAS remediation strategies. The officially recognized methods currently adopted in Japan mainly target PFOA, PFOS, and PFHxS in drinking water and environmental water. Looking ahead, we expect there will be increasing demand for regulations on longer-chain PFAS, leading to a greater focus on analytical methods that cover a wider range of PFAS compounds.’ Among environmental samples, water samples account for 60–70%, while soil makes up about 30%. In addition, exhaust gas from factories and waste are also analyzed.’ A European case study of 15 months of robustness A look to The Netherlands - HET Waterlaboratorium’s PFAS testing methodA look to The Netherlands - HET Waterlaboratorium’s 15 months of robustness. Eurofins Japan We have spoken to Ms Megumi Monden-san, Mr. Hayao Ogata-san, Mr. Tomoya Nojima-san and Miss Rosamond-san, and Ms. Machida-san from the environment testing group at Eurofins Nihon Kankyo. Having a reliable partner for method development is crucial. The collaboration between HET Waterlaboratorium and the SCIEX European support team exemplifies the importance of teamwork in achieving scientific excellence. Their combined expertise has resulted in a method that not only meets but exceeds industry standards, ensuring that HET Waterlaboratorium can continue to deliver high-quality results to their customers. Technical notes An ultra-high sensitivity analysis of PFAS compounds in multiple water sources PFAS analysis on the SCIEX 7500 system: 15 months of robustness data Megumi Monden Manager Hayao Ogata Associate Manager Eurofins Nihon Kankyo K.K. Environment testing Japan POPs (PFAS PCB) team Industry collaborations: a customer success story16 | sciex.com 17 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Adressing the challenges of PFAS testing 0418 | sciex.com 19 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Addressing the challenges of PFAS testing The challenges Addressing the challenges of PFAS testing20 | sciex.com 21 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Solutions at every level 0522 | sciex.com 23 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle The complete solution guide Software An easy to learn software system ensures fast result interpretation that is consistent and doesn’t create a bottleneck for your sample turnover. SCIEX OS qualitative rules (“traffic lights”) are used to quickly identify PFAS detections. Custom calculated columns tailored to EPA requirements are available to get you up and running fast. LC Built from the same legacy of innovation as all SCIEX products, these systems deliver precision and robustness with the assurance of quality and support you would expect from the leader in the quantification of molecules. Service Setting up PFAS testing from scratch requires a bit of tweaking in the beginning. When you are just starting out a reliable support team is as important as the system you purchase. SCIEX support specialists have years of PFAS experience under their belt and get your lab up to speed fast and for good. SCIEX 4500 system Sensitive and robust performance meets all EPA method 533 performance criteria but is mainly used in other environmental matrices than drinking water where the focus is on robust performance. ZenoTOF 7600 system Traditional fragmentation methods using collision-induced dissociation (CID) can be too aggressive to form diagnostic MS/MS spectra. The ZenoTOF 7600 system, electron activated dissociation (EAD) has shown potential as a form of fragmentation to produce more robust spectra for PFAS analysis. X500R QTOF system The greater selectivity from highresolution fragments provided cleaner chromatograms with lower background noise for more sensitive quantitation and increased analyte specificity for more confident identification. SCIEX 7500+ system For ultimate quantitation of trace level PFAS compounds, the SCIEX 7500+ system is the instrument of choice. SCIEX 6500+ system The LOQS of the European Drinking Water Directive are easily achievable with the QTRAP 6500+ system for all required PFAS compounds and without SPE. SCIEX 5500+ system Excellent sensitivity and precision to easily meet minimum reporting limits of EPA method 533 with excellent linear dynamic range.24 | sciex.com 25 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle SCIEX 7500+ system Enter the SCIEX 7500+ system, the mass spectrometer providing the highest sensitivity delivered by our instrument fleet to-date. Combined with reliable sample preparation steps and robust LC chromatography methods, the 7500+ not only delivers trace-level quantitation to meet the most demanding needs, but also tackles challenging matrices that were once thought to be impossible to test by LC-MS/MS. A few highlights before your download: • Mass Guard technology actively removed contaminating ions in complex matrices, which imparted exceptional robustness to the SCIEX 7500+ system • The SCIEX 7500+ system maintained quantitative performance after >7000 injections of food extracts and solvent QC samples with most PFAS analytes retaining >70% of the initial peak area sensitivity • The combination of SCIEX OS software enhancements for system performance tracking and the extractable DJet+ assembly offers increased flexibility for user-initiated management of system maintenance and uptime • Equipped with the renowned sensitivity of the SCIEX 7500 system, the exceptional data stability and robustness demonstrated by the SCIEX 7500+ system deliver a powerful and efficient platform for PFAS analysis in food Achieving exceptional robustness for PFAS analysis in food with the nextgeneration SCIEX 7500+ system. This technical note demonstrates >2x robustness improvement for the analysis of PFAS food extracts on the SCIEX 7500+ system. At the end of the study, comprising over 6400 food matrix injections, the majority of PFAS compounds (10 out 13) maintained >70% of the initial sensitivity. Residue analysis in food matrices is challenged by the presence of interfering coextractables which can result in instrument contamination and system downtime. Here, the robustness of the SCIEX 7500+ system and SCIEX 7500 system was evaluated in an accelerated manner through an aggressive sample preparation procedure and by omitting the diverter valve. The SCIEX 7500+ system features new Mass Guard technology designed to improve instrument robustness while maintaining optimal sensitivity longer. In the beginning of this eBook, we first asked the question: How low can we go? Regardless of where you are in the world, trace-level PFAS testing levels seem to be a pre-requisite for an application to be deemed suitable for challenging assays. 26 | sciex.com 27 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Reporting out on concentrations and amounts of analytes present in a given matrix is the basis of a targeted approach. However, as we are all aware, there are roughly 8000 to 12,000 potential PFAS compounds in existence, depending on how a family of analytes are classified based on their fluorinated state. A targeted MRM method simply cannot accommodate such a large number of compounds, especially when a large number of them have not even been identified. This is where a nontargeted approach, by the accurate mass route, becomes a valuable method of both discovery, identification, and ultimately quantitation. We present two applications that addresses different components of the PFAS lifecycle: PFAS characterization in cosmetic products, and then a demonstration of the power of EAD technology on the ZenoTOF 7600 system to decipher specific structures of PFAS molecules. Although these are non-targeted approached for analysis of PFAS from a discovery and structural analysis point of view, there remains a common goal of possessing the ability to quantify concentrations per unit of matrix for understanding various levels of PFAS contamination. Why do we need this when there is no current government regulations requirement for unknown PFAS discovery, you ask? The answer lies in the future of PFAS applications, we should prepare and be ready for anything coming our way, so allow SCIEX to help you achieve that goal. Characterizing PFAS in cosmetic products using non-targeted acquisition and Molecular Profiler Software - Leverage Data-Dependent Acquisition (DDA) with the ZenoTOF 7600 system to characterize PFAS compounds - Suspect screening and confirmation by library matching against the SCIEX Fluorochemical HR-MS/MS Spectral Library can produce good initial compound identification data - Molecular Profiler, the software, identifies PAPs-like properties with diagnostic fragment ion screening results in significant time-savings Use of electron activated dissociation (EAD) to elucidate PFAS structures - The EAD approach collecting MS/MS spectra generally can generate more fragments to help confirm compound identity during a non-targeted analysis - Ramping energy ranges over a set time can product unique fragments exclusive to a particular class of compounds, providing additional spectral information for the identification of nontargeted PFAS structures So far, we have spent a large amount of time discussing the merits of quantitation, and trace-level testing of PFAS compounds driven by sensitivity and accuracy. These advantages are provided by a targeted approach where the mass spec user is fully aware of the specific list of compounds and analytes they are targeting for both identification and quantitation. SCIEX ZenoTOF 7600 system 28 | sciex.com 29 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle SCIEX 6500+ system If certain regional regulations of PFAS-testing do not require the absolute trace-levels of low sensitivity quantitation, then this is an ideal and proven platform to bestow your trust upon. Here we highlight a PFAS application in drinking water, employing the technique of direct injection and detection by LCMS/MS. Baseline PFAS contamination can be reduced to a minimum to ensure the capture of high quality MSMS spectra, while the power and flexibility of the SCIEX OS software will enable your lab to adhere to regional requirements such as the European Union (EU)’s Directive 2020/2184. Automated solid-phase extraction system for the analysis of PFAS in drinking water. This technical note demonstrates the use of the PromoChrom automated solid-phase extraction (SPE) system for the analysis of PFAS in drinking water following EPA Method 533. Using the SCIEX QTRAP 6500+ system, negligible background contamination was observed as well as excellent method performance in spikes into reagent water and raw untreated groundwater samples. Milli-Q water blank spikes at 2, 40 and 70 ng/L showed mean recovery ranging from 96% to 115% with the mean precision <10% coefficient of variation (CV). Sample matrix and duplicate spikes at 2 and 40 ng/L showed mean recovery between 95% and 122% with <13%CV. Analysis of raw untreated groundwater samples showed the detection of 5 out of the 6 EPA-regulated PFAS compounds. One of our most popular ‘workhorse’ instruments ever built, the QTRAP 6500+ system continues to perform – handling large numbers of injections with ease and reliability. 1 Craig M. Butt1, Lily Sanchez2, Prem Parmar2, Sam Lodge3 1 SCIEX, USA; 2 Orange County Water District, Fountain Valley, CA; 3 Phenomenex, USA This technical note demonstrates the use of the PromoChrom automated solid-phase extraction (SPE) system for the analysis of PFAS in drinking water following EPA Method 533. Using the SCIEX QTRAP 6500+ system, negligible background contamination was observed as well as excellent method performance in spikes into reagent water and raw untreated groundwater samples. Milli-Q water blank spikes at 2, 40 and 70 ng/L showed mean recovery ranging from 96% to 115% with the mean precision <10% coefficient of variation (CV). Sample matrix and duplicate spikes at 2 and 40 ng/L showed mean recovery between 95% and 122% with <13%CV (representative chromatograms shown in Figure 1). Analysis of raw untreated groundwater samples showed the detection of 5 out of the 6 EPA-regulated PFAS compounds. Key benefits of the PromoChrom automated SPE system for the analysis of PFAS in drinking water • Automated sample extraction. Reduced sample preparation time through the fast, reproducible extraction and clean-up of drinking water samples • Low system background contamination. Quality control blanks predominantly showed non-detectable PFAS levels • Excellent method performance in quality control spikes. Method performance was evaluated with spikes into Milli-Q water and raw untreated groundwater samples • Real-world water samples. 10 raw untreated groundwater samples analyzed to demonstrate method applicability Automated solid-phase extraction system for the analysis of PFAS in drinking water Figure 1. Representative extracted ion chromatograms (XICs) in a 2 ng/L laboratory fortified sample matrix (LFSM) sample for the 6 EPA-regulated PFAS compounds. Raw, untreated groundwater was used for the LFSM sample. 30 | sciex.com 31 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Our 5500+ suite of mass spectrometers are capable for meeting two of the guidelines set out by the institution. Here we present how both the EPA 533 and EPA 1633 method are delivered using the 5500+ system. Key Features: • Existing methods were adapted to meet challenges of novel PFAS compounds • Minimum reporting limits of 2 ng/L with excellent linear dynamic range were achieved • Method showed good peak and chromatographic resolution of all compounds The combination of sample preparation, and well-designed LC chromatography, opens up some possibilities around the type of hardware needed for some specific requirements set out by the EPA. SCIEX 5500+ system p 1 EPA method 533 for PFAS analysis in drinking water at low parts-per-trillion levels Using the SCIEX Triple Quad™ 5500+ LC-MS/MS System – QTRAP® Ready Craig M. Butt1, Karl A. Oetjen1, Thep Phomsopha2 1 SCIEX, USA; 2 Eurofins ETA West Sacramento, USA This application note describes PFAS drinking water analysis by EPA Method 5331 using the SCIEX Triple Quad 5500+ LCMS/MS System – QTRAP Ready. Excellent sensitivity and precision were shown. The “in-sample” minimum reporting limits were 2 ng/L for all analytes except PFHpA (4 ng/L). Figure 1 shows MRM chromatograms for the novel perfluorinated ether carboxylic and sulfonic acids in the 0.50 ng/mL standard, which corresponds to 2 ng/L in sample. These values are significantly below the US EPA drinking water guidelines of 70 ng/L for PFOS and PFOA. Use of the custom built calculations and flagging rules within the SCIEX OS Software were used to streamline data review and report generation. EPA Method 533 builds upon the previously published EPA Methods 537 and 537.1, but with notable differences. Several odd-chain PFSAs, short-chain PFCAs, FTS compounds and novel perfluoroether carboxylates and sulfonates were added, whereas the FOSAA acids (NEtFOSAA, NMeFOSAA) and longchain PFCAs (PFTA, PFTrDA) were excluded. Structures of the novel compounds are shown in Figure 2. Similar to previous EPA methods, water samples are concentrated using solid-phase extraction (SPE) cartridges, but the choice of cartridge is flexible and the sample volume can vary from 100-250 mL. In addition, Method 533 incorporates the use of stable isotope dilution standards to minimize matrix effects and improve data quality. Key features of EPA method 533 on the SCIEX 5500+ System • Existing methods were adapted to meet challenges of novel PFAS compounds • Minimum reporting limits of 2 ng/L with excellent linear dynamic range were achieved • Method showed good peak and chromatographic resolution of all compounds • Data review and report generation was simplified through use of SCIEX OS Software custom calculations and flagging rules Figure 1. MRM chromatograms for novel perfluorinated ether acids. MRM XICs for the novel perfluorinated ether acids are shown from the 0.50 ng/mL in-vial standard (2 ng/L in sample equivalent). EPA method 533 for PFAS analysis in drinking water at low parts-per-trillion levels PFAS drinking water analysis by EPA Method 5331 using the SCIEX 5500+ System. Excellent sensitivity and precision were as shown; the “insample” minimum reporting limits were 2 ng/L for all analytes except PFHpA which was 4 ng/L. Novel perfluorinated ether carboxylic and sulfonic acids were detected in 0.50 ng/mL standard, which corresponds to 2 ng/L in sample, significantly below the US EPA drinking water guidelines of 70 ng/L for PFOS and PFOA. Custom built calculations and flagging rules in SCIEX OS Software streamlined data review and report generation. 32 | sciex.com 33 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle The EPA method 537.1 was one of the first EPA regulation specifically identifying a certain number of PFAS compounds needing to be tested in a single mass spectrometry method. SCIEX 4500 system Compound Abbreviation Method detection limit (ng/mL) UCRM3 reporting limit (ng/mL) Perfluorohexane carboxylate PFHxA 0.09 - Perfluoroheptane carboxylate PFHpA 0.1 10 Perfluorooctane carboxylate PFOA 0.1 20 Perfluorononane carboxylate PFNA 0.09 20 Perfluorodecane carboxylate PFDA 0.1 - Perfluoroundecanecarboxylate PFUnDA 0.1 - Perfluorododecane carboxylate PFDoA 0.1 - Perfluorotridecane carboxylate PFTrDA 0.2 - Perfluorotetradecane carboxylate PFTeDA 0.2 - Perfluorobutane sulfonate PFBS 0.1 90 Perfluorohexane sulfonate PFHxS 0.08 30 Perfluorooctane sulfonate PFOS 0.1 40 n-ethyl perfluorooctane sulfonamidoacetic acid n-EtFOSAA 0.1 - n-methyl perfluorooctane sulfonamidoacetic acid n-MeFOSAA 0.09 - In this case, the QTRAP 4500 system, was used and proved to be sufficient to quantify 14 PFAS compounds in drinking water, rounding out the entire SCIEX mass spectrometer suite to highlight that there is a different solution for any requirement you might need. Key Features: • Robust and reproducible results with qualifying accuracy and precision for calculated concentrations, asymmetry factor, and linearity • Total sample runtime takes only 8-10 min, depending on autosampler settings and system dead volume • Sensitive MDLs of 0.08-0.2 ng/L for the entire suite of 14 PFAS compounds Analysis of PFAS in drinking water with EPA method 537.1 In order to protect the safety of drinking water and human health, the EPA releases methods for the detection of contaminants. The EPA method 537.1 describes the detection of selected perand polyfluorinated alkyl substances in drinking water. Here a robust LC-MRM assay was developed using the QTRAP 4500 system for PFAS detection. Sensitive MDLs of 0.08-0.2 ng/L for all of 14 PFAS compounds in EPA method 537 were achieved, all of which meet or exceed the requirements of the US EPA’s UCMR3 list in a 10-minute run. 34 | sciex.com 35 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Controlling carryover with the ExionLC AE system Background levels for PFAS were less and 1/3 of the lower concentration standard (1ppt or 1pg/mL), less than 1% variation for mean CVs, and much more. Check out how the ExionLC AE system can enable you to do just that: Key Features: • Low system carryover: Limit carryover using the ExionLC AE system to <1/3 of the calculated maximum residue limit (MRL) for PFAS testing • Negligible system background: Attain background blank samples consistently <1/3 of the lowest concentration standard (1 ppt) • Repeatability across injections: Obtain consistent results across 55 injections with an average %CV value of 3.1% across all compounds tested While the solutions presented here so far are hardware driven from the mass spectrometer perspective, there are some distinct advantages available through the liquid chromatography system that provide an extra level of analysis, especially when it comes to minimizing carryover from sample to sample, and reducing background contamination. Controlling carryover and background contamination in PFAS analysis using the ExionLC AE system In this technical note, the combined use of the ExionLC AE system and the ExionLC AE PFAS kit demonstrated negligible system background and low system carryover, which enabled sensitive and precise quantitation of per- and polyfluoroalkyl substances. Having an HPLC system that contains minimal PFAS contamination is crucial for ensuring the accuracy and reliability of analytical results. PFAS, known for their persistence and environmental concerns, can contaminate HPLC equipment, leading to inaccurate data and potential misinterpretation of results. An HPLC system with limited PFAS contamination and low background levels helps prevent inaccurate results, aids detection and ensures compliance with increasingly stringent regulations related to PFAS use. 36 | sciex.com 37 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle SCIEX OS software: when software compliments hardware 0638 | sciex.com 39 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle SCIEX OS: when software compliments hardware Users want to load their samples and push a button—without the need to monitor the system until data are acquired, processed and ready for review—and during data review, they want to be able to easily identify outliers and failed samples. SCIEX OS software brings this vision to life with an easy-to-use interface and automated batch-building tools. It also provides automated customizable decision rules that immediately determine what to do with a sample that fails acceptance criteria and automated data processing and sample flagging rules. While Analyst software was the flagship data acquisition and processing software for SCIEX triple quadrupole and QTRAP systems, SCIEX OS software is the platform of the future, bringing all SCIEX mass spectrometers under a single software for acquisition and processing. With advanced tools that streamline and automate workflows like never before, and data security with built-in 21 CFR Part 11 compliance tools, SCIEX OS software can transform the way you work. The technical debt incurred by not maintaining up-to-date software can be detrimental to the overall efficiency of the lab. With regular cadence updates to SCIEX OS software, driven by the feedback we gain from our users through various channels, we strive to continue to serve our customers in the best way possible. Mass spectrometry has become the gold standard solution for quantitative analytical assays in many applications, from PFAS testing to pharmaceutical drug research and development. Software plays a key role in all these applications, because without it, we can’t drive the instrument or process the data it generates. SCIEX OS calculated columns and custom flagging for PFAS applications: EPA methods 533 and 1633 Engineered to do more. Faster. The integrated software platform solution for all SCIEX innovations, SCIEX OS software delivers data integrity, seamless usability and efficiency gains for your mass spectrometry workflows throughout your laboratory. Built on advanced and sophisticated algorithms, SCIEX OS software facilitates instrument control and automated data processing, simplifying your workflows and empowering swift, well informed decision-making. This technical note demonstrates the formulation of several quality control (QC) calculations and flagging rules directly within the SCIEX OS software for EPA PFAS Methods 533 and 1633. Using the Calculated Columns feature in the processing method, SCIEX OS eliminates the need to export the data to a thirdparty software platform, minimizing data processing and review time. In addition, the development of Custom Flagging rules within SCIEX OS allows for the quick review of data outside of the EPA criteria. The flexibility of SCIEX OS is shown, highlighting the ability to adapt to changing QC requirements. 1 Craig M. Butt1, Megumi Shimizu1, Karl Oetjen1 SCIEX, USA This technical note demonstrates the formulation of several quality control (QC) calculations and flagging rules directly within the SCIEX OS software for EPA PFAS Methods 533 and 1633. Using the Calculated Columns feature in the processing method, SCIEX OS eliminates the need to export the data to a third-party software platform, minimizing data processing and review time (Figure 1). In addition, the development of Custom Flagging rules within SCIEX OS allows for the quick review of data outside of the EPA criteria. The flexibility of SCIEX OS is shown, highlighting the ability to adapt to changing QC requirements. Key benefits of using SCIEX OS calculated columns and custom flagging for EPA PFAS methods 533 and 1633 • Flexibility to build QC calculations for EPA PFAS methods. Calculated Columns feature in SCIEX OS was used to build extensive QC equations for EPA methods 533 and 1633; calculation output directly within Results Table • Rapidly identify out-of-range QC samples. Custom Flagging rules were developed in SCIEX OS to flag QC samples that were outside of acceptance criteria range • Data processing and review time saved. Ability to formulate QC calculations and flagging rules directly in SCIEX OS reduces the time spent on data processing and review SCIEX OS calculated columns and custom flagging for PFAS applications: EPA methods 533 and 1633 Figure 1. Screenshots of the Calculated Columns and Flagging Rules features in SCIEX OS April Quinn-Paquet Global Marketing Product Manager, Software 40 | sciex.com 41 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle 07 PFAS around the world: regional focus and trends42 | sciex.com 43 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle PFAS around the world: regional focus and trends North America PFAS around the world Europe Karl Oetjen Market development Manager, Americas This rule marks a significant milestone in the U.S. and has major implications for the Americas, as other countries continue to address PFAS and develop their own regulations. In response, there is now a heightened urgency among U.S. public water systems to align with these new standards. It’s estimated that 6-10% of the 66,000 public drinking water systems nationwide may need to take action to reduce PFAS levels to comply with these regulations. They are preparing to undertake comprehensive monitoring over the next three years and developing strategies to mitigate any exceedances of PFAS compounds within five years. Additionally, we have observed a notable increase in PFAS soil testing in our region. As awareness of PFAS contamination grows, stakeholders are not only focusing on drinking water but also on the broader environmental impact of these chemicals. Soil testing has become a critical component in identifying and mitigating PFAS contamination at its source, helping to prevent further spread to water supplies and agricultural products. This comprehensive approach is essential for effectively managing PFAS pollution and protecting both public health and the environment. The scope of analytes to be quantified includes compounds listed in the EU Commission Recommendation, EU 2022/1431. The Commission Regulation EU 2022/2388 was followed to ensure that enforced limits are met for the relevant PFAS compounds mentioned. These regulations have been driving the demand for testing with high sensitivity, selectivity and reliability. SCIEX experts, in collaboration with users and thought leaders, have been able to continuously improve our solutions and provide optimized support for our customers. Besides tap water and environmental water, there are individual needs such as the development of PFAS purification systems and the measurement of PFAS in wastewater. Given the anticipated strengthening of regulations worldwide and the extensive variety of PFAS, estimated to be around 5000 types, there could be a demand for both targeted and non-targeted PFAS measurements. Confident quantification of per - and polyfluoroalkyl substances in water intended for human consumption. The recent announcement of the EPA’s final testing limits for PFAS marks the introduction of the United States’ first-ever national, legally enforceable drinking water standard aimed at protecting communities from exposure to these harmful substances. PFAS compounds are now considered to be of major concern due to their inherent bio-accumulation potential. This concern has become apparent to regulators who are increasingly extending testing requirements for these compounds, which is impacting food manufacturers and producers. Dan McMillian Senior Market Development Manager, EMEAI 44 | sciex.com 45 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle PFAS around the world China PFAS around the world Japan PFOA, PFOS, and PFHxS have been listed as the key controlled new pollutants, which prohibits their production, processing, use, import, and export. China’s new Standards for Drinking Water Quality (GB 5749-2022) set limits for PFOA and PFOS in tap water at <80 ng/L and 40 ng/L, respectively. This regulation represents the first Chinese guideline of PFAS in drinking water employing LC-MS/MS. Meanwhile, the government will strengthen PFAS source prevention and control, with a particular focus on construction projects in key industries such as petrochemicals, coatings, textile printing and dyeing, rubber, pesticides, pharmaceuticals, electroplating, and tanning. With the continuous improvement of technology and policies, China strives to effectively control PFAS pollution and promote the sustained improvement of ecological and environmental quality. However, in June 2024, the Food Safety Commission of Japan conducted a health impact assessment of perfluoroalkyl substances (PFAS) and determined that a TDI (tolerable daily intake) of 20 ng/kg body weight/day for both PFOS and PFOA is appropriate. As a result, this is now considered the standard for monitoring PFAS in food. Additionally, investigations involving the collection of concentration distribution data for PFAS in drinking water, food, and other potential exposure sources are expected to be conducted in the future. Besides tap water and environmental water, there are individual needs such as the development of PFAS purification systems and the measurement of PFAS in wastewater. Given the anticipated strengthening of regulations worldwide and the extensive variety of PFAS, estimated to be around 5000 types, there could be a demand for both targeted and non-targeted PFAS measurements. The Chinese government has released the “Action Plan for the Treatment of New Pollutants,” aiming to address PFAS pollution through investigation, monitoring, risk assessment, and whole-process control. Currently in Japan, provisional target values for PFOA and PFOS have been established for tap water and environmental water, but the measurement is not mandatory. Haiyan Cheng Senior Market Development Manager, China Kai Uchiumi Market Development Manager, Japan 46 | sciex.com 47 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle PFAS around the world Southeast Asia PFAS around the world Australia and New Zealand Despite lacking strict regulations in most nations, Singapore stands out for its proactive approach. The Singapore Food Agency (SFA) diligently monitors PFAS levels, setting stringent limits aligned with global standards. Employing cutting-edge technology like liquid chromatography-tandem mass spectrometry (LC-MS/MS), SFA ensures accurate and sensitive detection of PFAS compounds in diverse food samples. Their findings, particularly in seafood, underscore their commitment to consumer safety. While current levels pose minimal risk, ongoing surveillance and alignment with international standards remain paramount. For the broader ASEAN region, SeeChung Yip and his SEA application team from SCIEX offer invaluable support and consultation for PFAS testing in food, ensuring a concerted effort to address this critical health concern. Asia Summit: PFAS testing in the East There are now PFAS-contaminated sites around Australia resulting from these various uses. Over time, the chemicals have worked their way across and through the soil to contaminate surface and ground water, and have migrated into adjoining land areas. PFAS are also present in waste streams, including at landfills and wastewater treatment facilities, and more broadly in the environment. The PFAS National Environmental Management Plan (PFAS NEMP), developed by all state, territory and the Australian Governments, as well as the New Zealand Government, through HEPA’s National Chemicals Working Group, provides nationally agreed guidance and standards on the investigation, assessment and management of PFAS wastes and contamination in the environment, including prevention of the spread of contamination. The final PFAS NEMP 2.0 was agreed by Heads of EPAs in October 2019 and published in May 2020. A NEMP 3.0 has been drafted and the Nation Chemical Working Group has received feedback from the public, which is expected to be finalised in 2024. The new guidance focuses on the following SIX areas: 1. PFAS family - international approaches to grouping of PFASs 2. Environmental data and monitoring guidance on ambient monitoring data collection and land use classifications to enable comparability 3. Water-risk-based criteria and guidance for beneficial reuse of biosolids 4. Soil - guidance and standards around PFAS behaviour in soil, including leaching and associated ecological and human health guidance. It finalises and reviews two guideline values already in the NEMP and proposes two new guideline values for soil and one for wildlife diet 5. Resource recovery and waste guidance on management of risks associated with PFASin resource recovery products 6. Site specific guidance - guidance on principles and approaches to remediation and management; guidance on construction water; and guidance on estuarine, coastal and marine sediment PFAS Testing in food: Safeguarding consumer health in the wider Asia region. The presence of PFAS chemicals in food is an emerging concern across ASEAN countries, with recent studies revealing varied contamination levels. In Australia and New Zealand, PFAS have been used for a long time in a wide range of consumer products and industrial applications, including certain firefighting foams. The Australian Industrial Chemicals Introduction Scheme (AICIS) provides information on PFASs. See Chung Yip Field Application and Market Development Manager Charlie Liu Field Applications and Market Development Specialist 48 | sciex.com 49 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle After sales, service, and support: for all your needs 0850 | sciex.com 51 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Why choose SCIEX service? After sales, service, and support: for all your needs Ensure peak performance with SCIEX servicing and support • Maximize Uptime: Keep your lab productive with guaranteed onsite response, parts delivery, and remote monitoring services for a swift return to full operational status • Full SCIEX Coverage: Benefit from unparalleled expertise, parts availability, and training across the entire SCIEX portfolio of instruments, workflows, and software • Total Workflow Support: From instrument installations to relocations, software training, workflow validations, and more, SCIEX provides comprehensive support for your entire workflow Ensure your lab’s success with SCIEX’s dedicated servicing and support, designed to keep your PFAS testing system at peak performance. Discover a service package that meets your needs and budget by visiting SCIEX Instrument Service and Support Regular maintenance of both hardware and software is crucial for efficient laboratory operations. A well-serviced mass spectrometer system can achieve up to 18% higher productivity compared to one without a service plan. SCIEX offers a range of service plans and packages to support your SCIEX LC-MS/ MS systems throughout their lifespan. These plans include genuine parts, software, and expert assistance to meet your workflow needs. Whether you have a legacy instrument or the latest model, SCIEX service plans ensure consistent service, support, and satisfaction. For more information, visit SCIEX service. SCIEX Now • Manage your instruments. • Submit and manage support cases, track status and view history. • Access online training courses and articles. • Manage software licenses linked to your registered instruments. • View and report critical instrument statistics when connected to StatusScope remote monitoring service. • Be a part of the SCIEX community by submitting questions and comments. • Receive notifications from SCIEX with content based on your preferences. SCIEX Now learning hub • SCIEX Now learning hub success programs provide LC-MS and CE training customized to meet your exact needs. • With a selection of training methods and certifications available, you can build a mass spectrometry program that is most suited to your lab and users. • Starting with a clear understanding of your desired learning outcomes, we aim to help you improve lab productivity and consistency by designing and delivering a program that is focused on knowledge advancement and retention. SCIEX Now support network Maintaining and servicing your PFAS testing system Ensure peak performance with SCIEX servicing and support The success of your laboratory depends on several critical factors: the expertise of your staff, robust methodologies, and the reliability of your PFAS testing LCMS/MS system. In a constantly changing regulatory environment, it’s essential to keep your system running at its best. SCIEX servicing and support offer a comprehensive range of preventative maintenance services designed to minimize downtime, preventing costly sample backlogs and delays. 52 | sciex.com 53 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle After sales, service, and support: for all your needs Upskilling, refreshing and advancing your Team’s Knowledge SCIEX provides a comprehensive learning hub designed to enhance your team’s skills and knowledge. This hub offers a variety of free courses to help your team upskill immediately. Additionally, there are several paid options for onsite training with a SCIEX expert or hands-on experience in a SCIEX classroom at a regional location. Exclusive features of the SCIEX Learning hub: • Tailored technology: Enhance training retention with a personalized mix of online, in-person courses, and hands-on experience • Flexible training options: Learn at your own pace online, receive training at one of SCIEX’s global facilities or at your site • Unlimited course access: Enroll to gain unlimited access to over 300 courses, with no time restrictions or additional commitments • Centralized training management: Easily browse the course catalog, enroll in courses, track your progress, and print transcripts and certificates—all from a single login Additional benefits of upskilling for PFAS testing using LC-MS/ MS with SCIEX: • Unmatched analytical precision: With SCIEX’s cutting-edge LC-MS/ MS technology, your team will achieve unparalleled accuracy and reliability in PFAS quantitation, setting new standards in analytical performance. • Enhanced contamination control: Our training programs include best practices to help minimize background PFAS contamination, ensuring your results are consistently precise. • Regulatory mastery: Stay ahead of the curve with the latest techniques and regulatory updates. SCIEX training ensures your team meets and exceeds stringent environmental and health standards for PFAS testing. • Operational excellence: Empower your team to optimize workflows and troubleshoot with ease. SCIEX-trained personnel work more efficiently, delivering faster and more effective PFAS analysis. • Professional growth: SCIEX’s commitment to continuous learning fosters professional development, keeping your team motivated, engaged, and at the forefront of their field. 54 | sciex.com 55 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle 09 On-demand: customer collaborations56 | sciex.com 57 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle On-demand: customer collaborations Phase I: PFAS testing: A scientific series Our inaugural event kicked off the scientific series soon after the 4ppq announcement from the EPA. Not only was SCIEX first to market with an application and technical presentation with Eurofins California, we also gathered 3 additional industry experts, complemented by our internal applications team, to deliver a userled roundtable. Click on the link to access all the on-demand materials! Phase II: PFAS in food testing with SCIEX OS software As the conversation of PFAS-testing gradually expands beyond drinking water, the next component with the PFAS lifecycle began to include PFAS in food, and food packaging materials. From farming, production, to consumption, food encompasses may aspects of our everyday lives, and information is needed at all levels to improve our understanding of its presence. By extension, human exposure is another area where we can start to evaluate the impact and effects of long-term PFAS exposure. All this, along with the advantages of SCIEX OS for your PFAS-testing needs, can be uncovered here in our second PFAS Summit. SCIEX PFAS summits: Throughout the last few years, SCIEX have hosted our very own PFAS Summits – Scientific Series. One of our goals was to provide an educational channel for all mass spec users to come to an online forum and exchange scientific ideas and technical knowledge, while providing a platform for our industry-leading collaborators to present their work in the PFAS-testing world to a global audience. Amy Rand Assistant Professor Carleton University Andrew Patterson Technical Director, Eurofins Specialty Services Cora Young Associate Professor and Guy Warwick Rogers Chair York University Christopher Higgins PhD, University University Distinguished Professor, Colorado School of Mines Pradeep Dewapriya Postdoctoral Research Fellow, The University of Queensland, Australia Xanthippe Theurillat R&D Specialist, Nestle, Switzerland Kevin Stroski PhD candidate, Baylor University Cheryl Murphy Professor and Director, Center for PFAS Research, Michigan State University, USA Christian Lindh Associate Professor and Senior University Lecturer, Lund University, Sweden Anthony Williams Scientist, Center of Computational Toxicology and Exposure, US Environmental Protection Agency (EPA) Andrew Savage Expert Chemist, NQAC, Dublin, OH, USA Yelena Sapozhn Expert Chemist, USDA, ARS, Wyndmoor, PA, USA Christel Nielsen Occupational and Environmental Medicine, Lund University, Sweden 58 | sciex.com 59 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle On-demand: customer collaborations Phase III: A day in the life of the PFAS lifecycle After Phase II of our PFAS Summit, our users were specifically requesting addition topics to be discussed around the PFAS lifecycle, as well as specific examples of ‘what good looks like’. For this event, we invited industry leaders from NIST, the FDA, post-doctoral researchers, to provide yet another unique perspective into other aspects of the detection and quantitation of forever chemicals. Amy Rand Assistant Professor, Charleton University, Canada Annelise Blomberg Postdoctoral Researcher, Lund University, Sweden Christian Lindh Associate Professor and Senior University Lecturer, Lund University, Sweden Larry Zintek Organic Methods Group Leader, US EPA Ben Place Research Chemist, National Institute of Standards and Technology (NIST) Jeremy Gauthier Postdoctoral Fellow, University of Toronto, Canada Pradeep Dewapriya Postdoctoral Research Fellow, Queensland Alliance of Environmental Health Sciences (QAEHS) Susie Genualdi Research Chemist, Food and Drug Administration (FDA) Yuki Liang Laboratory Technician, University of British Columbia, Canada 60 | sciex.com 61 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Technical materials 1062 | sciex.com 63 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Drinking water has been identified as a significant source of PFAS exposure. Contamination can be through nearby industrial plants – from AFFF-impacted soils and water – or from runoff from agricultural fields. A robust and sensitive routine analysis method of 40 PFAS compounds in surface water using the SCIEX 7500 system This technical note describes a sensitive and robust method for the analysis of per- and polyfluoroalkyl substances (PFAS) in surface water which is based on EU Directive 2020/2184 and WAC/IV/A/025 and is accredited under the ISO 17025. Automated solid-phase extraction system for the analysis of PFAS in drinking waters This technical note demonstrates the use of the PromoChrom automated solid-phase extraction (SPE) system for the analysis of PFAS in drinking water following EPA Method 533. 1 Craig M. Butt1, Lily Sanchez2, Prem Parmar2, Sam Lodge3 1 SCIEX, USA; 2 Orange County Water District, Fountain Valley, CA; 3 Phenomenex, USA This technical note demonstrates the use of the PromoChrom automated solid-phase extraction (SPE) system for the analysis of PFAS in drinking water following EPA Method 533. Using the SCIEX QTRAP 6500+ system, negligible background contamination was observed as well as excellent method performance in spikes into reagent water and raw untreated groundwater samples. Milli-Q water blank spikes at 2, 40 and 70 ng/L showed mean recovery ranging from 96% to 115% with the mean precision <10% coefficient of variation (CV). Sample matrix and duplicate spikes at 2 and 40 ng/L showed mean recovery between 95% and 122% with <13%CV (representative chromatograms shown in Figure 1). Analysis of raw untreated groundwater samples showed the detection of 5 out of the 6 EPA-regulated PFAS compounds. Key benefits of the PromoChrom automated SPE system for the analysis of PFAS in drinking water • Automated sample extraction. Reduced sample preparation time through the fast, reproducible extraction and clean-up of drinking water samples • Low system background contamination. Quality control blanks predominantly showed non-detectable PFAS levels • Excellent method performance in quality control spikes. Method performance was evaluated with spikes into Milli-Q water and raw untreated groundwater samples • Real-world water samples. 10 raw untreated groundwater samples analyzed to demonstrate method applicability Automated solid-phase extraction system for the analysis of PFAS in drinking water Figure 1. Representative extracted ion chromatograms (XICs) in a 2 ng/L laboratory fortified sample matrix (LFSM) sample for the 6 EPA-regulated PFAS 1 compounds. Raw, untreated groundwater was used for the LFSM sample. Liesel Claeys1, Fred van Geenen2, Kevin Privat3, Fien Van Daele1, Leen Vandekerckhove1, Said El Ouadi2, and Jianru Stahl-Zeng4 1VMM, Belgium, 2SCIEX, Netherlands, 3SCIEX, France, 4SCIEX, Germany This technical note describes a sensitive and robust method for the analysis of per- and polyfluoroalkyl substances (PFAS) in surface water which is based on EU Directive 2020/2184 and WAC/IV/A/025 and is accredited under the ISO 17025. Using the SCIEX 7500 system, a comprehensive method for 40 PFAS compounds was developed with limits of detection (LODs) ranging from 0.5 to 5 ng/L and limits of quantitation (LOQs) ranging from 1 to 10 ng/L in surface water. The validation study showed good accuracy, precision and 4-week shelf life for all PFAS compounds. A thorough quality control program was implemented to ensure consistent data quality during the routine analysis. For example, the Shewhart chart for PFBS showed good accuracy and instrument stability for the 60 ng/L standard (see Figure 1). The use of the calculated columns and custom flagging rules in the SCIEX OS software resulted in fast, efficient data processing and review. Key benefits for PFAS analysis in surface water using the 7500 system • Accreditation achieved with the flexible scope of ISO 17025: The method was based on EU directive 2020/2184 and WAC/IV/A/025 • Comprehensive method for PFAS in surface water: The analyte panel covered 40 PFAS compounds, including 6 compounds that were reported as their total (branched + linear) and linear isomers • High levels of sensitivity: Surface water LODw values between 0.5 – 5 ng/L and LOQw values between 1 – 10 ng/L • Efficient data processing and review: SCIEX OS software calculated columns and automated flagging rules were integrated into the comprehensive quality control program to streamline data analysis, achieving a 50% reduction in data analysis time A robust and sensitive routine analysis method of 40 PFAS compounds in surface water using the SCIEX 7500 system Figure 1: Shewhart control chart of 60 ng/L PFBS in surface water. PFAS analysis on the SCIEX 7500 system: 15 months of robustness data Demonstrates the robustness of the SCIEX 7500 system over 15 months of routine PFAS analysis with various water samples. EPA method 533 for PFAS analysis in drinking water at low parts-per-trillion levels Excellent sensitivity and precision were as shown; the “in-sample” minimum reporting limits were 2 ng/L for all analytes except PFHpA which was 4 ng/L. Simultaneous quantitation of ultrashort-, short- and long-chain PFAS in water by a single direct injection LC-MS/MS method This technical note describes a direct injection LC-MS/MS method for the simultaneous quantitation of ultrashort-, short-and long-chain per- and polyfluoroalkyl substances (PFAS). p 1 For research use only. Not for use in diagnostics procedures. PFAS analysis on the SCIEX 7500 system: 15 months of robustness data Kay Hup1, Abdessamad Chahbouni1, Jack Steed2, Bertram Nieland3, Said El Ouadi3, Daniel McMillan2 and Jianru Stahl-Zeng4 1Het Waterlaboratorium; 2SCIEX, UK; 3SCIEX, The Netherlands; 4SCIEX, Germany This technical note demonstrates the robustness of the SCIEX 7500 system over 15 months of routine PFAS analysis with various water samples. Quality control (QC) samples, spiked at 10 ng/L with L-PFHxS, L-PFOS, L-PFOA and L-PFNA, showed accuracies generally within ±1 standard deviation of the mean and all QC samples were with 30% of the mean values (Figure 1). Only 1 preventative maintenance (PM) service was performed during the 15-month timeframe. During the analysis, approximately 100–200 injections were performed per week and other non-PFAS applications were also run. These results highlight the strong robustness of both the analysis method and the SCIEX 7500 system. A robust analysis is paramount to the long-term viability of routine PFAS analysis. In this technical note, the developed method was validated for 26 PFAS compounds of interest in LCMS-grade, drinking, ground and surface water samples.1 Modifications were made to the LC system to reduce background contamination, including replacing or bypassing any components of the system that contribute to PFAS contamination. Specifically, system components containing fluorinated ethylene propylene (FEP) and Teflon were bypassed or replaced with polyether ether ketone (PEEK), when possible. Key benefits of long-term PFAS analysis using the SCIEX 7500 system • Long-term stability of QC samples with no loss in sensitivity: Robustness demonstrated by all QC samples within ±30% of the mean over 15 months • Minimal maintenance: Preventive maintenance was only performed once during the 15-month period. Prior to the preventive maintenance, the calibration specifications were met with only front-end cleaning required. • Diversity of water samples analyzed: Several different water matrices were analyzed, including ground, surface and drinking water Figure 1. Percent accuracy plots of 4 regulated PFAS compounds at multiple timepoints. The plots highlight the robustness observed. The grey dotted lines show ±1 standard deviation and the green dotted lines show ±3 standard deviations. During this period, no value fell outside of ±30% of the mean. The QC samples were spiked into matrix and were representative of multiple different water samples. 10 ng/L L-PFOA 10 ng/L L-PFHxS 10 ng/L L-PFNA 10 ng/L L-PFOS p 1 EPA method 533 for PFAS analysis in drinking water at low parts-per-trillion levels Using the SCIEX Triple Quad™ 5500+ LC-MS/MS System – QTRAP® Ready Craig M. Butt1, Karl A. Oetjen1, Thep Phomsopha2 1 SCIEX, USA; 2 Eurofins ETA West Sacramento, USA This application note describes PFAS drinking water analysis by EPA Method 5331 using the SCIEX Triple Quad 5500+ LCMS/MS System – QTRAP Ready. Excellent sensitivity and precision were shown. The “in-sample” minimum reporting limits were 2 ng/L for all analytes except PFHpA (4 ng/L). Figure 1 shows MRM chromatograms for the novel perfluorinated ether carboxylic and sulfonic acids in the 0.50 ng/mL standard, which corresponds to 2 ng/L in sample. These values are significantly below the US EPA drinking water guidelines of 70 ng/L for PFOS and PFOA. Use of the custom built calculations and flagging rules within the SCIEX OS Software were used to streamline data review and report generation. EPA Method 533 builds upon the previously published EPA Methods 537 and 537.1, but with notable differences. Several odd-chain PFSAs, short-chain PFCAs, FTS compounds and novel perfluoroether carboxylates and sulfonates were added, whereas the FOSAA acids (NEtFOSAA, NMeFOSAA) and longchain PFCAs (PFTA, PFTrDA) were excluded. Structures of the novel compounds are shown in Figure 2. Similar to previous EPA methods, water samples are concentrated using solid-phase extraction (SPE) cartridges, but the choice of cartridge is flexible and the sample volume can vary from 100-250 mL. In addition, Method 533 incorporates the use of stable isotope dilution standards to minimize matrix effects and improve data quality. Key features of EPA method 533 on the SCIEX 5500+ System • Existing methods were adapted to meet challenges of novel PFAS compounds • Minimum reporting limits of 2 ng/L with excellent linear dynamic range were achieved • Method showed good peak and chromatographic resolution of all compounds • Data review and report generation was simplified through use of SCIEX OS Software custom calculations and flagging rules Figure 1. MRM chromatograms for novel perfluorinated ether acids. MRM XICs for the novel perfluorinated ether acids are shown from the 0.50 ng/mL in-vial standard (2 ng/L in sample equivalent). Holly Lee1, Simon Roberts2, Craig M. Butt2, Sam Lodge3, RenXi Ye4, Cora Young4 and Trevor VandenBoer4 1SCIEX, Canada; 2SCIEX, USA; 3Phenomenex, USA; 4York University, Canada This technical note describes a direct injection LC-MS/MS method for the simultaneous quantitation of ultrashort-, shortand long-chain per- and polyfluoroalkyl substances (PFAS). in water. Mixed-mode chromatography demonstrated robust retention and separation for the wide range of PFAS chain lengths tested. The sensitivity of the SCIEX 7500 system enabled in-sample limits of quantitation (LOQs) of 0.2–10 ng/L and method detection limits (MDLs) of 0.1–13 ng/L for most target analytes. TFA, PFBA, 5:3 and 7:3 FTCAs, and 6:2 and 8:2 diPAP required higher LOQs (10–100 ng/L) due to background contamination. Application of the method to tap water, rainwater and lake water revealed the predominance of TFA at sub-to-low µg/L levels (Figure 1). Key benefits of the SCIEX 7500 system for analyzing ultrashort-, short- and long-chain PFAS • Robust retention and separation for a wide range of PFAS chain lengths: Extensive chromatographic optimization enabled stable retention times (RTs) for the ultrashort-chain PFAAs and excellent separation from the void region. • Accurate and reproducible quantitation at the LOQ: Mean accuracy (±25%) and precision (%CV <25%) were achieved at sub-to-low ng/L LOQs for most target PFAS. • Good quantitative performance in tap water spikes: Recoveries of 80–120% and precision %CV <20% for most of the target PFAS were achieved in tap water spiked at 3 different concentrations. • Detection in different aqueous matrices: Sub-ng/L to µg/L levels of PFAAs were detected in real-world tap water, rainwater and lake water. Simultaneous quantitation of ultrashort-, short- and long-chain PFAS in water by a single direct injection LC-MS/MS method Figure 1. Quantitation of TFA in real-world aqueous matrices. Representative extracted ion chromatograms (XICs) of TFA demonstrate its ubiquity at sub-µg/L levels in tap water, surface water and rainwater. Water64 | sciex.com 65 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle PFAS are used in many of our consumer goods, such as food packaging papers, cosmetics, personal care products, nonstick cookware, textiles, furniture, stain repellant sprays and cleaning products. Quantitation of per- and polyfluoroalkyl substances (PFAS) in textiles This technical note describes the analysis of per- and polyfluoroalkyl substances (PFAS) in textiles using the SCIEX 6500+ system. Leveraging high-resolution mass spectrometry (HRMS) for PFAS quantitation and resolving interferences in food matrices This technical note describes a LC-MS/MS method for the simultaneous quantitation and identification of PFAS in food on the ZenoTOF 7600 system. Holly Lee1 and Craig M. Butt2 1SCIEX, Canada; 2SCIEX, USA This technical note describes an LC-HRMS method for the simultaneous quantitation and identification of PFAS in food using the ZenoTOF 7600 system. The selectivity from HRMS acquisition mass-resolved PFAS from their interferences, resulting in more confident compound confirmation in complex food matrices (Figure 1). Matrix spikes demonstrated acceptable method performance for most analytes at target LOQs set by food testing authorities and below the regulated maximum residue limits (MRLs). The instrument sensitivity from ZenoMRMHR acquisition also enabled a small injection volume of 3 µL and solvent-based calibration to minimize matrix effects, while still achieving sub-ppb limits of quantitation (LOQs). Key benefits of the ZenoTOF 7600 system for analyzing PFAS in food matrices • Mass-resolving matrix interferences: HRMS selectivity enabled more confident PFAS detection by mass-resolving co-eluting interferences in food matrices. • Matrix recoveries meeting target criteria: >85% of the analyte/matrix combinations tested met the recovery and repeatability performance requirements established by food testing authorities • Leveraging ZenoMRMHR sensitivity for quantitation: Reduced matrix effects from smaller injections enabled the use of solvent-based calibration, while achieving sub-ppb LOQs for quantitation. Leveraging high-resolution mass spectrometry (HRMS) for resolving PFAS interferences and quantitation in food matrices Figure 1. The power of high-resolution mass spectrometry for removing matrix interferences in food. Comparison of representative extracted ion chromatograms (XICs) acquired on a nominal (top) and accurate (bottom) mass spectrometer demonstrates how the higher selectivity from the latter can be used to significantly improve the detection of PFBA and PFPeA by removing co-eluting matrix interferences in a 0.15 µg/kg corn snaplage spiked extract. Sabarinathan1, Sashank Pillai1, Craig M. Butt2 1SCIEX, India; 2SCIEX, USA This technical note describes the analysis of per- and polyfluoroalkyl substances (PFAS) in textiles using the SCIEX 6500+ system. In-sample equivalent limits of quantitation (LOQs) ranged between 25 pg/g and 125 pg/g except for PFBA (5000 pg/g) and NFDHA (1250 pg/g). Matrix spikes were performed at 0.25, 5 and 25 ng/g using a cotton shirt that did not contain background PFAS levels, Overall, the matrix spikes showed excellent recovery (95.4–131%) and precision (%CV 3.1– 28%) at the 0.25 ng/g spiking level. The method was applied to four locally purchased clothing pieces. PFPeA, PFHxA, 4:2 FTS, and 6:2 FTS were detected in the clothing at low ng/g levels. Key benefits of the SCIEX 6500+ system for PFAS quantitation in textiles • Mid-range pg/g sensitivity using the SCIEX 6500+ system: In-sample equivalent LOQs ranged from 25 to 125 pg/g for all target PFAS, except for PFBA (5000 pg/g) and NFDHA (1250 pg/g). • Good quantitative performance in matrix spikes: Matrix spikes at 5 and 25 ng/g demonstrated recoveries of 100±10% and precision %CV <10%. The 0.25 ng/g spike showed accuracy from 95% to 131% and precision %CV <28%. • Method applicability in purchased clothing: Low ng/g levels of PFPeA, PFHxA, 4:2 FTS, and 6:2 FTS were detected. Quantitation of per- and polyfluoroalkyl substances (PFAS) in textiles Figure 1. Extracted ion chromatograms (XICs) of PFPeA, PFHxA, 4:2 FTS and 6:2 FTS detected in clothing sample #1. Characterizing PFAS in cosmetic products using non-target acquisition and Molecule Profiler software. This technical note outlines the analysis of PFAS in cosmetics using non-targeted acquisition (NTA) with compound identification through suspect screening and diagnostic fragment ion confirmation. Achieving exceptional robustness for PFAS analysis in food with the next-generation SCIEX 7500+ system This technical note demonstrates >2x robustness improvement for the analysis of PFAS food extracts on the SCIEX 7500+ system. Quantitation of per- and polyfluoroalkyl substances (PFAS) in foodstuffs This technical note describes a simple and sensitive method using the SCIEX 7500 system for the quantitation of per- and polyfluoroalkyl substances (PFAS) in different foodstuffs. 1 Craig M. Butt1, Mikyanny Reyes1, Holly Lee2, Keegan Harris3 and Amy Rand3 1SCIEX, USA; 2SCIEX, Canada; 3Carleton University, Canada This technical note outlines the analysis of PFAS in cosmetics using non-targeted acquisition (NTA) with compound identification through suspect screening and diagnostic fragment ion confirmation (Figure 1). The ZenoTOF 7600 system used data-dependent acquisition (DDA) to obtain TOFMS precursor and TOFMSMS fragmentation spectra. SCIEX OS software was used for initial compound identification through library matching suspect analytes with the SCIEX Fluorochemical HR-MS/MS Spectral Library. Additional manual screening showed the presence of several PAPs-like compounds, known ingredients in certain cosmetic products. The Molecule Profiler software was employed to rapidly find precursor compounds that shared a diagnostic PAPs fragment ion, reducing the time to detect structurally similar novel PFAS in the cosmetics samples. Key benefits of PFAS characterization in cosmetics using the ZenoTOF 7600 system • Rapid filtering of non-targeted acquisition results for positive detections. SCIEX OS qualitative rules (“traffic lights”) are used to quickly identify PFAS detections • Improved confidence in PFAS identification through MS/MS library matching. SCIEX Fluorochemical HR-MS/MS Spectral Library was used to confirm identification by comparison to the library database • Detection of novel PFAS compounds through diagnostic fragment ion screening in Molecule Profiler. Rapid screening of non-targeted data sets to discover new PFAS Characterizing PFAS in cosmetic products using non-targeted acquisition and Molecule Profiler software Figure 1. Instrumental and data processing workflow for the characterization of PFAS in cosmetics. Holly Lee, Ian Moore, Craig M. Butt and Elliott Jones SCIEX, Canada; SCIEX, USA This technical note demonstrates >2x robustness improvement for the analysis of PFAS food extracts on the SCIEX 7500+ system. At the end of the study, comprising over 6400 food matrix injections, the majority of PFAS compounds (10 out 13) maintained >70% of the initial sensitivity. Residue analysis in food matrices is challenged by the presence of interfering coextractables which can result in instrument contamination and system downtime. Here, the robustness of the SCIEX 7500+ system and SCIEX 7500 system was evaluated in an accelerated manner through an aggressive sample preparation procedure and by omitting the diverter valve. The SCIEX 7500+ system features new Mass Guard technology1 designed to improve instrument robustness while maintaining optimal sensitivity longer. Key benefits of high-throughput PFAS analysis in food using the SCIEX 7500+ system • Enhanced robustness from Mass Guard technology: Improved hardware components to reduce downstream instrument contamination, maintaining instrument uptime • Exceptional instrument stability: The SCIEX 7500+ system achieved >2x improvement in robustness, as demonstrated by >6400 injections of food matrices, compared to >3000 injections on the SCIEX 7500 system • User-accessibility via an extractable DJet+ assembly: Increased flexibility for user cleaning when required Achieving exceptional robustness for PFAS analysis in food with the next-generation SCIEX 7500+ system Figure 1. Raw peak areas normalized to initial response (A) and internal standard (IS)-corrected peak area ratios (B) for perfluorooctane sulfonate (PFOS) in solvent quality control (QC) samples on the SCIEX 7500 (blue) and on the SCIEX 7500+ (green) systems. Each datapoint represents the mean with standard error bars. In panel A, the dotted lines represent the 100% and 50% raw peak areas relative to the initial response. Robustness was compared based on the total number of injections before the instrument sensitivity declined to 50% of the maxima. In panel B, the dotted lines represent the overall mean and %CV for each experiment. Food extracts were injected between each solvent QC datapoint. 1000 2000 3000 4000 5000 6000 7000 0.00 0.05 0.10 0.15 0.20 0.25 1000 2000 3000 4000 5000 6000 7000 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 IS-corrected area ratio PFOS 1 Normalized raw peak areas Injections 1000 2000 3000 4000 5000 6000 7000 0.00 0.05 0.10 0.15 0.20 0.25 1000 2000 3000 4000 5000 6000 7000 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 IS-corrected area ratio PFOS 1 Normalized raw peak areas Injections 3054 matrix injections on 7500 6480 matrix injections on 7500+ A B 8.0 %CV 11 %CV SCIEX 7500+ system SCIEX 7500 system F F F F F F F F F F F F F F F F F SO3H Injections p 1 For research use only. Not for use in diagnostics procedures. Quantitation of per- and polyfluoroalkyl substances (PFAS) in foodstuffs Michael Scherer1, Jessica Smith2, Jack Steed2, Daniel McMillan2, Jianru Stahl-Zeng1 1SCIEX, Germany; 2SCIEX, UK This technical note describes a simple and sensitive method using the SCIEX 7500 system for the quantitation of per- and polyfluoroalkyl substances (PFAS) in different foodstuffs. The method is in response to the new maximum residue levels (MRLs) outlined in the Commission Regulation (EU) 2022/2388 of 7 December 2022.1 The high sensitivity of the SCIEX 7500 system2 enabled the development of an LC-MS/MS method that requires only a 2 µL food extract injection volume, while still achieving good quantitative performance in the sub µg/kg range. Application of this method to the analysis of pork liver, honey and egg extracts provided by Fera Science Ltd. resulted in excellent agreement with the previously measured reference levels. PFAS compounds can enter the food chain either through environmental contamination or migration from food packaging. Based on a risk assessment of PFAS contamination in food on human health, the European Food Safety Authority (EFSA) established a group tolerable weekly intake (TWI) of 4.4 ng/kg body weight for the sum of PFOS, PFOA, PFNA and PFHxS. As a result, MRLs and total limits of the four PFAS were set, to regulate their presence in certain foodstuffs of animal origin as a protective measure against dietary exposure.1 Due to the lack of data for many foods, the Commission also recommended continued PFAS monitoring in a broad range of foodstuffs to assess the need for further regulatory actions.3 PFAS measurements in foods require low limits of quantitation (LOQs),4 which necessitate robust analytical performance and increased instrument sensitivity. Here, the sensitivity of the SCIEX 7500 system was leveraged to allow small sample injection volumes to reduce matrix interferences and to allow the use of solvent-based calibration to simplify quantitation for a wide variety of different food matrices. Key features of PFAS analysis in foodstuffs using the SCIEX 7500 system • The sensitivity of the SCIEX 7500 system allowed for a small injection volume of 2 µL to reduce matrix interferences in food extracts, while still achieving sub µg/kg LOQs based on signal-to-noise (S/N). • Acceptable precision (%CV <15%), linearity (r2 >0.995) and ion ratio tolerance (±30%) were achieved using the external solvent-based standard calibration curve. • Calculated concentrations for PFAS compounds in an EURL proficiency test sample (pork liver) were found to be within the satisfactory range (±2 z-score) • Positive detection of PFAS was achieved in the unspiked blank food extracts, although the levels were all below their corresponding MRLs Figure 1. Extracted ion chromatograms (XICs) of the 4 regulated PFAS compounds (PFOS, PFOA, PFNA and PFHxS) with their concentrations measured in an unspiked pork liver extract. Using the SCIEX 7500 system, LOQs of 0.01 ng/mL were achieved for PFOS and PFNA, and 0.02 ng/mL for PFHxS and PFOA, in diluent. This was based on an ion ratio tolerance of ±30% for the quantifier and qualifier transitions and S/N >10. Because of the small injection volume of 2 µL, the reduction of matrix effects in food enabled the use of solvent-based calibration to derive these low LOQs, which in turn allowed for positive detections of PFAS in even the unspiked food extracts. PFOS PFOA PFNA PFHxS 1. Sample preparation 2. Small volume direct injection 3. Sensitive and reproducible quantitation 0.38 µg/kg 0.06 µg/kg 0.09 µg/kg <LOQ Food and consumer goods 66 | sciex.com 67 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Human exposure Human exposure to PFAS occurs through multiple exposure pathways, including the ingestion of contaminated drinking water and food. Inhalation of indoor air and household dust, and dermal uptake from cosmetics and personal care products. People & PFAS: Quantitation of PFASs in human serum and blood using volumetric absorptive microsamplers (VAMS) This technical note describes the trace level analysis of per- and polyfluoroalkyl substances (PFAS) using only 60 µL of whole blood collected with VAMS devices. Analysis of per- and polyfluoroalkyl substances (PFAS) in aqueous, solid, biosolid and tissue samples following EPA Method 1633. This technical note demonstrates the performance of EPA Method 1633 for the analysis 40 PFAS in surface water, soil and fish tissue. p 1 For research use only. Not for use in diagnostics procedures. People and PFAS: Quantitation in human serum and blood using volumetric absorptive microsampling (VAMS) Courtney C. Carignan,1 Rachel A. Bauer,1 Andrew Patterson,2 Thep Phomsopha,2 Eric Redman,2 Heather M. Stapleton3 and Christopher P. Higgins4 1Michigan State University, USA; 2Eurofins Environment Testing Northern California, USA; 3Duke University, USA; 4Colorado School of Mines, USA This technical note describes the trace level analysis of per- and polyfluoroalkyl substances (PFAS) using only 60 µL of whole blood collected with volumetric absorptive microsampling (VAMS) devices (Figure 1). The sensitivity of the SCIEX 7500 system was used to achieve serum detection limits ranging from 0.1 to 1.0 ng/mL, which are sufficient for PFAS biomonitoring in the general population. National Institute of Standards and Technology (NIST) SRM 1957 samples that were collected using different sampling techniques were analyzed. These results demonstrated that samples collected with the VAMS method can be analyzed accurately and produce comparable results to samples collected by traditional PFAS serum sampling techniques. The use of VAMS for PFAS blood analysis overcomes many of the logistical obstacles common for traditional methods, such as the need for a trained phlebotomist for sample collection, sample storage and shipping costs. Key features of the method for PFAS analysis of blood and serum samples • Elevated sensitivity of the SCIEX 7500 system allowed for 100 pg/mL minimum detection levels, which are aligned with concentrations that are relevant for human health • Excellent recovery for both serum and VAMS sample preparation approaches, with average recoveries of 88% and 99%, respectively • The accuracy of the VAMS approach demonstrates an ability to support large-scale PFAS biomonitoring programs Figure 1. Graphical abstract (left) and comparison of PFOS content (right) in the method blank sample (MB, purple) and laboratory control sample (LCS, green). p 1 For research use only. Not for use in diagnostics procedures. Analysis of per- and polyfluoroalkyl substances (PFAS) in aqueous, solid, biosolid and tissue samples following EPA Method 1633 Megumi Shimizu1, Craig M. Butt1, Matt Noestheden1, Karl A. Oetjen1, Sam Lodge2 and Phil Bassignani3 1SCIEX, USA; 2Phenomenex, USA; 3Alpha Analytical, Inc, USA This technical note demonstrates the performance of EPA Method 1633 for the analysis 40 PFAS in surface water, soil and fish tissue. Using the SCIEX 5500+ system, initial demonstration of capability (IDC) experiments yielded experimental method detection limit (MDL) concentrations lower than the finalized, pooled values for aqueous matrices. Method robustness was demonstrated across 40 hours of extracted matrix and solvent standard injections. Mean accuracy ranged from 88% to 111% and the mean %CV was 4.9%. Further, the method achieved ~3 min resolution of TDCA from PFOS and PFHxS, which is a critical requirement of EPA Method 1633. Finally, analysis of sludge and soil standard reference materials (SRMs) showed comparable concentrations to their certified values, demonstrating good method accuracy. EPA Method 1633 method is an isotope dilution method that is comparable to drinking water PFAS methods (EPA Methods 533 and 537.1). In addition to the compounds in EPA Methods 533 and 537.1, EPA Method 1633 includes long chain perfluorinated sulfonic acids (PFNS, PFDS, PFDoS), fluorooctanesulfonamides (FOSAs), fluorooctanesulfonamidoethanols (FOSEs) and x:3, fluorotelomer carboxylic acids (FTCAs). Unlike the previous EPA PFAS methods, EPA Method 1633 requires monitoring 2 fragment ions for most analytes. Key benefits of the analysis following EPA Method 1633 on the SCIEX 5500+ system • The observed limits of quantitation (LOQ) were 0.1x to 0.5x of the EPA level 1 standard (Figure 1), except for PFOSA • The method showed chromatographic separation of taurodeoxycholic acid (TDCA) from PFOS (>2 min) and other PFAS analytes • The method showed excellent robustness across ~40 hours of 125 continuous injections of solvent standards and matrix samples. The mean accuracy of the continuing calibration verification (CCV) standard (n=10) was 98%. • The accurate quantitation with real-world samples was demonstrated using SRMs Figure 1. LOQ chromatograms for representative PFAS compounds. In-vial LOQ concentrations were 0.1x to 0.5x lower than the level 1 EPA standard, demonstrating the high sensitivity of the method. The chromatograms shown cover the diverse range of PFAS classes included in EPA Method 1633. 68 | sciex.com 69 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle 11 Phenomenex: your partner in PFAS testing consumables70 | sciex.com 71 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Phenomenex: your partner in PFAS testing consumables Our list of solutions include: • Standardization and Calibration • Sample preparation • Analytical columns • Testing Applications • Complimentary full-time support from experts Bringing robustness, efficiency, and quality data to your PFAS analysis Phenomenex is our sister company within Danaher that provides high-quality and costeffective chromatography PFAS analytical tools, PFAS testing methods, and resources to help you and your lab achieve quality analysis in a wide range of PFAS matrices. New! “Designed for PFAS” Complete product portfolio Phenomenex now provides new QC tested SPE plus a vast selection of consumables verified for PFAS analysis, reduce potential risk of false positives due to background contamination. To order PFAS products and learn more, visit www.phenomenex.com/PFAS Designed for PFAS Complete product portfolio aiming to reduce or eliminate background interferences • PFAS QC tested SPE media • Sub-components verified for the absence of PFAS • Low background contamination 1501671696_DA0924_w_e1 The “Designed for PFAS” products offer reproducibility and accuracy in detecting and quantifying a broad range of PFAS compounds. From sample preparation to analysis, the “Designed for PFAS” portfolio has shown to meet the most stringent quality standards and maintain data quality without having to worry about background contamination. Click on the tab to find out more. 72 | sciex.com 73 The forever changing world of PFAS testing PFAS the global headline maker: regulations from around the world The PFAS lifecycle: an overview Industry collaborations: a customer success story Solutions at every level PFAS around the world: regional focus (MDM) and trends On-demand: customer collaborations Phenomenex: your partner in PFAS-testing consumables Addressing the challenges of PFAS testing SCIEX OS software: when software compliments hardware After-sales, service, and support: for all your needs Technical materials for each component of the PFAS lifecycle Conclusion Insustry experts, research leaders, internal application scientists, we present PFASIndustry experts from all our collaborators with different perspectives in the hope of enabling the wider scientific community to find the methodology and solution that fits their needs. Here at SCIEX, we understand and empathize the challenges many laboratories face when it comes to detecting and quantifying this family of forever chemicals. Whether it is trace-level detection at the parts-per-quadrillion level, the difference in matrices and therefore sample preparation steps, or simply the number of analytes needed to be included in the MRM list, it can be daunting. We hope you enjoyed our presentation of this eBook, and follow us online at our various channels to get the updates on what the SCIEX team is researching. For all the latest technical materials and resources Stay up to date and join the conversion The SCIEX clinical diagnostic portfolio is For In Vitro Diagnostic Use. Rx Only. Product(s) not available in all countries. For information on availability, please contact your local sales representative or refer to https://sciex.com/diagnostics. All other products are For Research Use Only. Not for use in Diagnostic Procedures. 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