Kai Zhang1. 1. U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Office of Regulatory Science, 5001 Campus Drive, College Park, MD 20740, USA.
Abstract
BACKGROUND: In the present study, we developed a novel automated sample preparation workflow for the determination of mycotoxins in foods. OBJECTIVE: This workflow integrates off-line devices such as a centrifuge, shaker, liquid and solid dispensing units into a unified platform to perform gravimetric and volumetric dispensing, capping/decapping, extraction, shaking, filtration, and centrifugation. Two robotic arms provide sample transportation without human assistance. METHOD: Critical method performance attributes were characterized using spiked corn, milk and peanut butter containing aflatoxins, deoxynivalenol, fumonisins, ochratoxin A, HT-2 and T-2 toxins and zearalenone and certified reference materials. Prepared samples were analyzed by liquid chromatography mass spectrometry (LC-MS). RESULTS: Recoveries of spiked samples range 100-120% with RSD<20% and the majority of measured values of certified reference materials are consistent with certified values within ±20%. Within- and between-batch variabilities of QC samples range 5-9% and 7-12% respectively. CONCLUSIONS: Our workflow introduces a straightforward and automated sample preparation procedure for LC-MS-based multimycotoxin analysis. Further, it demonstrates how individual sample preparation devices, that are conventionally used off-line, can be integrated together. HIGHLIGHTS: This study shows automated sample preparation will replace manual operations and significantly increase the degree of automation and standardization for sample preparation. AOAC INTERNATIONAL 2020. This work is written by a US Government employee and is in the public domain in the US.
BACKGROUND: In the present study, we developed a novel automated sample preparation workflow for the determination of mycotoxins in foods. OBJECTIVE: This workflow integrates off-line devices such as a centrifuge, shaker, liquid and solid dispensing units into a unified platform to perform gravimetric and volumetric dispensing, capping/decapping, extraction, shaking, filtration, and centrifugation. Two robotic arms provide sample transportation without human assistance. METHOD: Critical method performance attributes were characterized using spiked corn, milk and peanut butter containing aflatoxins, deoxynivalenol, fumonisins, ochratoxin A, HT-2 and T-2 toxins and zearalenone and certified reference materials. Prepared samples were analyzed by liquid chromatography mass spectrometry (LC-MS). RESULTS: Recoveries of spiked samples range 100-120% with RSD<20% and the majority of measured values of certified reference materials are consistent with certified values within ±20%. Within- and between-batch variabilities of QC samples range 5-9% and 7-12% respectively. CONCLUSIONS: Our workflow introduces a straightforward and automated sample preparation procedure for LC-MS-based multimycotoxin analysis. Further, it demonstrates how individual sample preparation devices, that are conventionally used off-line, can be integrated together. HIGHLIGHTS: This study shows automated sample preparation will replace manual operations and significantly increase the degree of automation and standardization for sample preparation. AOAC INTERNATIONAL 2020. This work is written by a US Government employee and is in the public domain in the US.