Analytical Quality by Design (AQbD) for Developing a Validated High-Performance Thin Layer Densitometry Method for Estimating Mangiferin in Human Plasma
Poster Apr 16, 2015
Rajneet Kaur Khurana, Atul Jain, OP Katare, Bhupinder Singh
Of late, Analytical Quality by Design (AQbD) has been gaining increased acceptance in the industrial, academic and regulatory circles. Considered as a science and risk-based approach, AQbD provides rational understanding of the critical method parameters (CMPs) affecting the critical analytical attributes (CAAs) of an analytical method. The present work aims at systematic development of a simple, rapid and highly sensitive bioanalytical high-performance thin-layer densitometry method for the analysis of mangiferin. Initially, the quality target method profile (QTMP) was defined and critical analytical attributes (CAAs) were earmarked. Preliminary studies were conducted for selecting the suitable mobile phase mixture, followed by primary and secondary screening studies employing D-optimal design and Plackett-Burman design, respectively for selecting the ideal mobile phase composition and prioritizing the critically influential method parameters on the CAAs. The CAAs chosen included retardation factor (Rf), peak height, capacity factor, theoretical plates and separation number. Response Surface Methodology (RSM) was conducted as per the face centered cubic design (FCCD) for optimizing volume loaded and plate dimension as the critical method parameters (CMPs) selected initially from the screening studies. The mobile phase containing mixture of ethyl acetate: acetic acid: formic acid: water in 7:1:1:1, v/v/v/v ratio was finally selected as the optimized combination owing to apt chromatographic separation for mangiferin at 262 nm with Rf 0.68±0.02, with all other parameters being within the acceptance limits. Method validation studies revealed high linearity for mangiferin in the concentration range of 50–800 ng/band with r2 =0.998 ± 0.005. The developed method showed high accuracy, precision, ruggedness, robustness, specificity, sensitivity, selectivity, recovery, detection limit (12.1 ng/band) and quantification limit (36.6 ng/band). The bioanalytical method for analysis of mangiferin in plasma revealed the presence of well-resolved peaks and high recovery of mangiferin.
Using Elemental Analysis For Discrimination Of Pinot Noir Wines From Six Different Districts In An AvaPoster
The determination of geographical origin of wine is gaining increased interest by researchers and federal agencies around the world, partially due to increased fraud with regards to place of origin labelling. For wine, multi-elemental profiling of macro, micro, and trace elements has been proposed for determination of authenticity. Commercial wines from different wineries in 5 different neighborhoods within one AVA show characteristic elemental fingerprints. Macro, micro and trace elements as well as elemental ratios contribute to the observed separation, indicating the involvement of multiple factors and underlying mechanisms, including location and soil composition, elemental uptake by vine and rootstock, viticulture and nutrient management, water sources, and small differences in the different wineries.READ MORE
Fast arsenic speciation analysis of wines and rice with LC-ICP-QQQPoster
This method was designed in response to recent and proposed food standards, both international and national, that limit inorganic arsenic rather than total, organic, or individual arsenic species such as arsenite (AsIII) and arsenate (AsV). Analysis time is 10x faster than the current FDA regulatory method, increasing sample throughput, avoided spectral interferences and dramatically increased sensitivity. Validation data from two laboratories demonstrate the method’s accuracy and reproducibility of both wine and rice matrices in a single analytical batch.READ MORE
Overcoming the Challenges of Analysing Ionic Polar Pesticides in FoodPoster
Here, the novel application of the Waters’ Torus DEA column is presented, showing the improved performance of a UPLC-MS/MS method for the underivatised
analysis of glyphosate and a selection of other anionic pesticides.