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A Collaborative Study: Determination of Mycotoxins in Corn, Peanut Butter, and Wheat Flour using Stable Isotope Dilution Assay (SIDA) and Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) Kai Zhang, Matthew R. Schaab, Gavin Southwood, Elizabeth R. Tor, Linda S. Aston, Wenlu Song, Brian David Eitzer, Sanghamitra Majumdar, Theodore Lapainis, Huy Mai, Kevin Tran, Aref ElDemerdash, Victor Vega, Yanxuan Cai, Jon W Wong, Alexander J. Krynitsky, and Timothy H. Begley J. Agric. Food Chem., Just Accepted Manuscript • DOI: 10.1021/acs.jafc.6b04872 • Publication Date (Web): 16 Dec 2016 Downloaded from http://pubs.acs.org on December 20, 2016
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Journal of Agricultural and Food Chemistry
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A Collaborative Study: Determination of Mycotoxins in Corn, Peanut Butter, and Wheat
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Flour using Stable Isotope Dilution Assay (SIDA) and Liquid Chromatography-Tandem
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Mass Spectrometry (LC-MS/MS)
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Kai Zhang*,†, Matthew R. Schaab‡, Gavin Southwood‡, Elizabeth R. Tor§, Linda S. Aston§,
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Wenlu Song#, Brian Eitzer┴, Sanghamitra Majumdar┴, Theodore Lapainis⊗, Huy Mai∇, Kevin
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Tran∇, Aref El-Demerdash∇, Victor Vega△, Yanxuan Cai∥, Jon W. Wong†, Alexandra J.
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Krynitsky†, Timothy H. Begley†
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†
U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Office of
Regulatory Science. 5001 Campus Drive, College Park, MD 20740
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‡
Arizona Department of Health Services. 250 N. 17th Avenue, Phoenix, AZ 85007.
§
California Animal Health and Food Safety Laboratory System. Toxicology Laboratory.
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West Health Sciences Drive, UC Davis, Davis, CA 95616
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California Department of Public Health, Food & Drug Lab Branch. 850 Marina Bay Parkway,
G365. Richmond, CA 94804
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┴
Connecticut Agricultural Experiment Station, Department of Analytical Chemistry. 123
Huntington Street, New Haven, CT 06511
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1 ACS Paragon Plus Environment
Journal of Agricultural and Food Chemistry
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⊗U.S.
Food and Drug Administration, Pacific Regional Laboratory Northwest. 22201 23rd Drive
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SE. Bothell, WA 98021.
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∇U.S.
Food and Drug Administration, Kansas City Laboratory. 11510 W. 80th Street, Lenexa,
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KS 66214.
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△U.S.
Food and Drug Administration, Southeast Regional Laboratory. 60 8th Street, Atlanta,
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GA 30309
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∥U.S.
Food and Drug Administration, Office of Regulatory Affairs. 12420 Parklawn Drive
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Element Building, Rockville, MD 20857.
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*To whom correspondence should be addressed; Tel: 240-402-2318;
[email protected];
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Journal of Agricultural and Food Chemistry
Abstract
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A collaborative study was conducted to evaluate stable isotope dilution assay (SIDA) and
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LC-MS/MS for the simultaneous determination of aflatoxin B1, B2, G1 and G2; deoxynivalenol;
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fumonisin B1, B2, B3; ochratoxin A; HT-2 toxin; T-2 toxin; and zearalenone in foods. Samples
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were fortified with twelve 13C uniformly labeled mycotoxins (13C-IS) corresponding to the native
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mycotoxins and extracted with acetonitrile/water (50/50: v/v), followed by centrifugation,
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filtration and LC-MS/MS analysis. In addition to certified reference materials, the six
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participating laboratories analyzed corn, peanut butter, and wheat flour fortified with the twelve
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mycotoxins at concentrations ranging from 1.0-1,000 ng/g. Using their available LC-MS/MS
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platform, each laboratory developed in-house instrumental conditions for analysis. The majority
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of recoveries ranged from 80-120% with relative standard derivations (RSDs) < 20%. Greater
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than 90% of the average recoveries of the participating laboratories were in the range of 90 -
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110%, with repeatability RSDr (within laboratory)
