Automate and Track Your Sample Preparation Workflow
How To Guide
Published: September 30, 2024
Credit: Thermo Fisher Scientific
Laboratories across industries including environmental testing, pharma and food safety rely heavily on gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) for precise analysis. However, sample preparation for these methods can be time-consuming and prone to errors, affecting both efficiency and data quality.
This eBook explores how a fully automated, traceable system can streamline GC and GC-MS workflows, enhancing accuracy and reducing errors.
Download this guide to discover:
- How automation boosts lab throughput and precision in GC and GC-MS workflows
- Strategies for minimizing manual errors and improving data quality
- The benefits of fully traceable sample preparation workflows
Easily program the Thermo Scientific™ TriPlus™ RSH SMART
Autosampler for integrated sample preparation with
operation traceability
Automate and track your
sample preparation workflow
Overcome the challenges of sample preparation
u TriPlus RSH SMART Autosampler with
Thermo Scientific™ ISQ™ 7610 Single Quadrupole
MS System coupled to Thermo Scientific™
TRACE™ 1610 Gas Chromatograph
Advantages of sample handling automation:
• Higher sample throughput
• Improved data repeatability
• Increased laboratory efficiency by
unattended routine operations
• Reduced cost per sample
• Enhanced confidence of the
analytical results
When gas chromatography (GC) or gas chromatography mass
spectrometry (GC-MS) analysis is performed, several manual
procedures are required in the laboratory to prepare the sample prior
to the injection, with the purpose of making it amenable to GC analysis,
or to increase sensitivity through analytes enrichment, or simply to
prepare standard solutions for instrument calibration.
Sample preparation normally involves multiple steps such as extraction,
clean up, dilution, standard addition, derivatization, mixing and heating.
More than 60% of the time spent in a chromatographic analysis can be
dedicated to sample preparation.
Additionally, it is estimated that approximately 30% of possible sources
of analytical error are due to manual sample handling (i.e., sample loss
and/or sample contamination), with significant consequences on the
analytical data accuracy and precision.
The Thermo Scientific™ TriPlus™ RSH SMART Autosampler is a
robotic platform enabling SMART technology for consumables ID
recognition and usage tracking. It is capable of combining highly
versatile sample introduction with automated and fully traceable sample
preparation procedures. The typical bottle-neck of manual GC and
GC-MS analytical workflows can be eliminated by this autosampler
through fully unattended operations and automated tracking of SMART
consumable usage, for increased confidence in the analytical results.
Basic and advanced sample preparation procedures can be performed
by batching samples before the GC analysis or sequentially by
optimizing the overall cycle time through overlapping capabilities.
Agitator/incubator for HS,
SPME or sample prep
Vortex mixer for
intensive sample mix
Barcode reader for
sample tracking
More sample trays
for higher capacity
SPME fiber
conditioning
for SPME
applications
Large volume
wash stations
Fast wash station
Large solvent station
Standard wash station
Centrifuge
Dilutor with
large reservoir
Controlled heating or
cooling of samples
Error-free sample handling
The Automatic Tool Change (ATC) provides the foundation
for automated basic and advanced sample handling and
sample preparation procedures. The automatic selection
of the suitable tool permits different injection techniques
like liquid, static and dynamic headspace, and solid phase
microextraction (SPME) to be executed within the same
sample sequence in a fully unattended way. Up to 6 different
tools can be programmed for extended sample preparation
capabilities. With that, different liquid syringes can be
dedicated to specific operations like standard addition or
dilution, minimizing possible cross contamination.
Several tools are available to reliably automate the most
common sample preparation procedures, including on-line
microSPE clean-up of QuEChERs extracts, and to achieve
the highest level of sample handling flexibility. Combined
with high sample capacity, the TriPlus RSH SMART
autosampler overcomes stringent productivity requirements.
SMART syringes and SPME/SPME Arrow fibers are
automatically recognized by the autosampler to further
streamline the workflow through error-free operations.
Additionally, the SMART technology allows to track
consumables usage and conditions, locally and through the
chromatography data system, supporting GLP accreditation.
Automated clean-up of QuEChERS extracts of foods
Evolve from manual clean-up operations to automated miniaturized cartridge-base µSPE
Automated µSPE clean-up available on the TriPlus RSH and TriPlus RSH SMART autosamplers allows modern laboratories
to gain reliable high throughput operations for GC-MS analysis of pesticides in a wide variety of food matrices, even those
with high lipid contents.
Replacing manual clean-up procedures with a fully automated on-line approach maintains the efficiency of the
QuEChERS extraction, while offering the benefits of eliminating human errors and scaling down sample volume
and solvent consumption.
The miniaturization of the clean-up step to a microliter scale solid-phase extraction prevents the typical dilution during
manual SPE operations, thus avoiding an additional evaporation step. The pesticides fraction is eluted only in a small
volume of a few 100 µL for direct injection into the GC-MS system.
Syringe accurately delivers
sample and solvents at the
desired volume and flow
Packed sorbent
maximizes the
separation efficiency
Needle guide eliminates
headspace above the
SPE sorbent
Crimped-on septum ensures
a closed flow path to the
SPE sorbent and facilitates
cartridge transport
Insertion of the syringe needle allows
delivery of sample and solvents
directly to the SPE sorbent
Higher selectivity and extended instrument up-time
Discover the benefits of the µSPE clean-up automated workflow
Unlike classical SPE using a vacuum manifold, the flow rate applied to the µSPE cartridge can be precisely controlled with
a liquid syringe on a TriPlus RSH autosampler, ensuring optimum selectivity and recovery.
The µSPE cartridge is sealed by a septum allowing the autosampler syringe to push the raw QuEChERS extract through
the sorbent bed. The syringe works as an LC pump. Low flow rates of approx. 2 µL/s in the load and elution steps are
used for sharp analyte/matrix separation.
Miniaturized SPE cartridges
Optimized sorbent
mix with minimum
dwell volume
Get 1 mL syringe
Discard µSPE cartridge
Get 100 µL syringe
Inject sample
START GC Analytical Run
START Next Sample Clean-up
Load 300 µL extract from vial
in Tray 1
Place mini-cartridge above
collection vial
Elute extract through µSPE
cartridge
Add 25 µL analyte protectant
and QC solution
• Automated workflow
Reduced manual errors and extended unattended operation
• Optimized sorbent material
Single type cartridge for hundreds of pesticides in many different food matrices
• Higher selectivity
Cleaner extract for an extended instrument uptime
• Miniaturization to microliter scale
Less sample and solvent consumption with no concentration step required
• Optimized cycle time through overlapping
Fast clean up step <10 min run in parallel to the chromatographic separation of the previous sample
>> visit thermofisher.com/microSPE to know more
Sequential dilution
A high concentration standard is automatically diluted
to easily meet your requirements.
Calibration dilution
Reliability and precision for your quantitative
calibration. Prepare calibration levels with or
without internal standards.
Standard addition
Add increasing amounts of standard to any sample.
Calibrating by standard additions is commonly used in
headspace and SPME analyses. The accurate addition
of standards is now a reliable, automated step in the
measurement cycle.
Sample derivatization
Derivatization steps for repeated batches of up to
six samples or sequentially for immediate injection to
prevent sample degradation.
Heating/mixing
Vials undergo automatic agitation after the addition
of standard volumes. You can also speed-up
headspace and SPME applications by reaching the
equilibrium faster.
Vortexing at ambient temperature
Physical vortexing for thorough mixing can be used
for liquid homogenization and extraction steps
with solvents.
Centrifugation
Essential tool for phase separation, supporting
automated liquid-liquid extraction with micro volumes.
Ambient temperature headspace
Perform static headspace injection skipping the
incubation step, for temperature sensitive samples
or for sampling from special vessels, i.e. Exetainer,®
Vacutainer.®
Ambient temperature SPME
Perform SPME injection skipping the incubation step,
for temperature sensitive samples.
Sequential dilution
Vortex mixer utilizing
different vial sizes
Centrifuge for phase
separation compatible
with flammable solvents
Incubator for mixing
and derivatization
Automated batch or
sequential derivatization
Calibration dilution with
internal standard
Let the robotic capabilities of the TriPlus RSH SMART
autosampler perform daily sample preparation workflow –
from samples and standards dilution up to more complex
derivatization protocols – automatically and reliably.
Actions such as sequential dilution, calibration dilution,
standard addition, batch and sequential sample
derivatization, heating/mixing and vortexing are now at
your fingertips to easily create your automated workflow.
Ready-to-use PrepCycles are pre-compiled set of basic
operations to go beyond standard injection functions and
are available within the TriPlus RSH SMART autosampler
as a default. Additionally, you can gain extra control of
your autosampler by programming customized workflows
to easily fulfill your routine sample handling needs.
Easily instruct the TriPlus RSH SMART
autosampler to perform daily sample
handling operations for you, in a fully
automated way, with the Thermo Scientific™
Sampling Workflow Editor software.
Simply connect the Sampling Workflow Editor software to
the TriPlus RSH SMART autosampler and all the configured
tools will be automatically recognized. Then, you can play
with all the actions compatible with your tools, through
an easy drag-and-drop approach, to program your own
sample preparation workflow.
Gain control of your TriPlus RSH SMART Autosampler
Sampling Workflow Editor
user interface. Intuitive
visual programming of
your autosampler through
drag-and-drop motion.
Visit www.thermofisher.com/SamplingWorkflowEditor to view the video demonstration.
10 mL of water sample into a 20 mL vial
Add Internal Standard (ISTD) and 2 mL of extraction solvent
Vortex vial
5 min waiting for phase separation
Large Volume Injection in the GC-MS/MS
10 mL of water sample into a 20 mL vial
Add Internal Standard (ISTD)
Add dispersive solvent (MeOH)
Add extraction solvent (DCM)
Vortex vial
Centrifugation
Transfer of the organic phase from vial bottom
Large Volume Injection in the GC-MS/MS
Automated liquid-liquid extraction (LLE) of Semi-Volatile
Organic Compounds (SVOC) in water samples
Semi-volatile organic contaminants in water belong to a wide variety of chemical
structures, such as hydrocarbons, pesticides, phenols, PCBs, PAHs and
nitrosamines, representing a serious risk for the environment and human health.
Liquid-liquid extraction remains one of the go-to options for organic contaminant
extraction from water samples, but manual operations are time consuming, prone to
human error, and involve high solvent consumption. Automated sample preparation
workflow coupled to the highly sensitive Thermo Scientific™ TSQ™ 9610 GC-MS/MS
is a valuable opportunity to save on solvent costs, minimize labor time, and achieve
extremely high data quality by removing the variability of manual operations.
Enhanced enrichment
Sensitivity at sub-ppt levels
On-line injection in the
GC-MS/MS system
Suitable for drinking, ground,
surface, sea water and wastewater
H24 operations
*www.SampleQ.com
*www.SampleQ.com
Dispersive liquid-liquid micro extraction (DLLME)
for sub-ppt sensitivity
The DLLME uses a micro volume of extraction solvent (ca 300 µL) added in a
dispersive way to water samples offering an elevated surface exchange, and
dramatically increasing the final concentration of the analytes in the organic phase.
Heptachlor
Peak at 0.5 ng/L
Endrin
Peak at 0.5 ng/L
Heptachlorepoxide
Peak at 0.5 ng/L
Heptenophos
Peak at 2.5 ng/L
Dibenzo (a,i) pyrene
Peak at 2.5 ng/L
p Quantified concentration in water samples
Simazine
Peak at 5 ng/L
In-vial extraction for limited sample
volume and solvent consumption
On-line injection in the
GC-MS/MS system
Suitable for drinking, ground,
surface, sea water and wastewater
Sensitivity at ppt levels
H24 operations
Boost sample preparation for environmental analysis
Automated DLLME workflow* steps
p Quantified concentration in water samples
Automated LLE workflow* steps
By eliminating the uncertainties of manual operations, this automated workflow enhances data precision
and provides greater confidence in quantitative results, all while adhering to regulatory requirements.
Suitable for the EPA 8260 compounds list, the TriPlus RSH SMART VOC Sample Prep Station is paired
with the Thermo Scientific ISQ 7610 Single Quadrupole GC-MS to achieve sensitivity at ppt level for VOCs
in water samples, ensuring high robustness and extended instrument uptime.
Liquid and headspace
tools move simultaneously
to allow the ISTD/SURR
addition just before vial
incubation and analysis,
maintaining headspace
cycle time optimization.
TriPlus RSH SMART VOC Sample Prep Station
u u u
An aliquot (10 mL) of water
sample is manually transferred
by the laboratory scientist into
20 mL HS vial
Vials are then placed
on the autosampler tray
Calibration solution addition QC solution addition (*optional)
ISTD / SURR addition ISTD /SURR addition
Vial Incubation Vial Incubation
GC Injection GC Injection
Calibration solution
preparation and analysis
Sample and QC
preparation and analysis
u Workflow for automated preparation of
calibration solutions and addition of IS/
Surrogate mix for the analysis of VOCs
Streamline Volatiles Organic Compounds (VOC) analysis for water and soil samples
The Thermo Scientific™ TriPlus™ RSH SMART VOC Sample Prep Station, in the dedicated dual-head configuration, streamlines
the headspace analysis of Volatile Organic Compounds (VOCs) in water and soil samples by automating sample preparation
steps and seamlessly integrating on-line HS-GC-MS analysis. This automated workflow preserves sample integrity by adding internal
standards and surrogates to samples just before headspace sampling and analysis, while maintaining overlap of all the steps for an
optimized cycle time. It also automates the preparation and analysis of calibration standards using the same procedure.
Thanks to the intelligent programming, the two heads can move simultaneously and synchronized, safely sharing a common
working space and optimizing the total cycle time for maximum sample throughput.
Visit thermofisher.com/triplusrshsmartvoc to know more
Streamlined control with Chromeleon CDS
Benefits of TriPlus RSH SMART
VOC Sample Prep workflow:
• Improve data quality with precision in
compliance with regulatory requirements
• Relieve manual operation and
enhance laboratory efficiency
through unattended operations
• H24 operations with highly
consistent results
• Facilitate good laboratory practice with
SMART consumables traceability and
instrument health notifications from
Thermo Scientific™ Chromeleon™
Chromatography Data System (CDS)
ISTD/surrogate peak area
%RSD across the samples
in the evaluation period of
six working days
The TriPlus RSH SMART VOC Sample Prep Station instrument control is fully integrated in Chromeleon 7.2.10
and 7.3 CDS, ensuring a smooth and efficient control of the automated workflow covering sequence setup, sample
preparation and online injection, data acquisition, and reporting.
The Chromeleon Environmental Analysis Extension Pack for EPA-based environmental applications provides a
comprehensive set of GC-MS e-workflows for quick sequence set-up and reporting templates to make data review
and reporting easier. Moreover, with the ever-evolving compliance requirements for data integrity and data security,
Chromeleon CDS offers a secure platform for analytical laboratories to comply with modern regulatory guidelines
including FDA 21 CFR Part 11 and European Commission (EU) Annex 11.
p
SIM trace showing the target compounds in a tap water sample spiked
with a VOC mix at the lowest calibration point (0.1 ng/mL). Calculated MDL
is ≤0.17 ng/mL for all the compounds (MDL for BTEX is 0.01 ng/mL).
The wide range of vials, septa, capillary columns and accessories offers applicationfocused solutions that are ideal for pharmaceutical, forensics/toxicology, environmental,
food analysis, petrochemical and general analytical industries.
Have you ever thought about the
quality of your glass vial? Especially
when you need to detect small
concentrations or certain structures
of analytes, it’s important to preserve
your sample integrity right from the
start with vials. With our SureSTART
brand you will find the vial best suited
for your needs. Find our offering in 3
different performance levels:
Performance Level 1: Everyday
applications; choose these for the
cost-effective choice
Performance Level 2: High throughput
applications; choose these when
robustness and reproducibility are key
Performance Level 3: High performance;
choose these when sensitivity is a must
All SureSTART products are
Specification Certified. In addition,
kits are either LC/GC Certified or
MS Certified.
Achieve error-free sample handling and electronic tracking capability using
Thermo Scientific™ SMART GC Syringes and SPME/SPME Arrow fibers with
the TriPlus RSH SMART Autosampler. Read/write ID chip on each field-proven
syringe and SPME fiber allows an automatic connection to the TriPlus RSH
SMART autosampler for information exchange. Key information such as part
number, lot number, usage parameters, operational ranges and history for
that specific consumable are stored in the chip. This information is directly
accessed and reported via Chromeleon CDS, integrating consumables
identification and usage tracking into an audit trail log file for GLP compliance.
The combination of smart syringe technology and Chromeleon CDS with the
TriPlus RSH SMART autosampler provides an entirely automated workflow for
full traceability in compliance with regulatory protocals.
Learn more about SureSTART
Learn more about GC SMART Syringes
Thermo Scientific chromatography consumables are designed to complement our
innovative range of GC and GC-MS systems together with our autosamplers. Get the most
out of the TriPlus RSH SMART autosampler by pairing it with advanced, high-performance
Thermo Scientific products.
SMART syringe chip for ID and
usage information storage
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presented as an example of the capabilities of Thermo Fisher Scientific products. It is not intended to encourage use of these products
in any manner that might infringe the intellectual property rights of others. Specifications, terms and pricing are subject to change. Not
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Learn more at thermofisher.com/triplusrsh
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