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ARS Home » Northeast Area » Wyndmoor, Pennsylvania » Eastern Regional Research Center » Microbial and Chemical Food Safety » Research » Publications at this Location » Publication #372076

Research Project: Development, Evaluation, and Validation of Technologies for the Detection and Characterization of Chemical Contaminants in Foods

Location: Microbial and Chemical Food Safety

Title: Evaluation of flow injection mass spectrometry approach for rapid screening of selected pesticides and mycotoxins in grain and animal feed samples

item Sapozhnikova, Yelena
item ZOMER, PAUL - Waneningen University
item GERSSEN, ARJEN - Waneningen University
item Nunez, Alberto
item MOL, HANS - Waneningen University

Submitted to: Food Control
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 4/25/2020
Publication Date: 4/30/2020
Citation: Sapozhnikova, Y.V., Zomer, P., Gerssen, A., Nunez, A., Mol, H.G. 2020. Evaluation of flow injection mass spectrometry approach for rapid screening of selected pesticides and mycotoxins in grain and animal feed samples. Food Control. 116.

Interpretive Summary: Fast and simple screening methods are needed for the analysis of harmful contaminants in food and feed samples in regulatory testing. In this study we developed and evaluated a novel screening approach based on mass spectrometry (MS) detection while eliminating chromatographic separation (flow injection MS) for selected pesticides and mycotoxins. The developed approach is fast (2 min) and straightforward, providing high throughput and lower cost. Limits of detection for the selected contaminants were assessed to meet their regulatory maximum residue levels in cereal/grain and animal feed samples. Additionally, we challenged MS without chromatography to separate pesticides structural isomers. Our results suggest that the new screening approach can be a useful tool for fast screening of multiple contaminants of various classes in complex food/feed samples.

Technical Abstract: A fast screening approach for simultaneous detection of twelve pesticides and seven mycotoxins in food and feed samples using flow injection (FI) mass spectrometry (MS) was developed and evaluated. Ten selected pesticides represented five pairs of structural isomers to challenge their MS differentiation without chromatographic separation. Samples of cereals/grains and animal feed were prepared using QuEChERS extraction, diluted and fortified with the selected contaminants to yield their representative maximum levels (MLs) or maximum residue levels (MRLs). Sensitivity of the developed approach was assessed for qualitative screening of the selected contaminants using triple quadrupole MS/MS and ion mobility (IM) HR-TOFMS. Despite the high complexity of the selected matrices and the absence of chromatography, limits of detection in fortified extracts were below established regulatory levels for 14 and 15 selected contaminants by FI-MS/MS and FI-IM-TOFMS analysis, respectively, in 36-100% samples. Experiments with ion mobility TOFMS did not result in successful separation of pesticide structural isomers. However, for three out of five pairs of pesticide structural isomers: cyproconazole and uniconazole, methiocarb and ethiofencarb, and vernolate and pebulate, unique fragment ions were found and confirmed with HR-QTOFMS for their MS differentiation. The developed approach is sensitive enough for rapid multi-residue screening of some pesticides and mycotoxins in complex samples of food and feed, providing high speed and throughput, simplicity and effective use of high-end instrumentation.