Determination of Aflatoxin B1 in Smokeless Tobacco Products by Use of UHPLC-MS/MS

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• 作者：Nicholas Zitomer ; Michael E. Rybak ; Zhong Li ; Matthew J. Walters ; Matthew R. Holman
• 刊名：Journal of Agricultural and Food Chemistry
• 出版年：2015
• 出版时间：October 21, 2015
• 年：2015
• 卷：63
• 期：41
• 页码：9131-9138
• 全文大小：337K
• ISSN：1520-5118

文摘

This work developed a UHPLC-MS/MS method for the detection and quantitation of aflatoxins in smokeless tobacco products, which was then used to determine aflatoxin B₁ concentrations in 32 smokeless tobacco products commercially available in the United States. Smokeless tobacco products were dried, milled, and amended with ¹³C₁₇-labeled internal standards, extracted in water/methanol solution in the presence of a surfactant, isolated through use of immunoaffinity column chromatography, and reconstituted in mobile phase prior to UHPLC-MS/MS analysis. The method was capable of baseline separation of aflatoxins B₁, B₂, G₁, and G₂ in a 2.5 min run by use of a fused core C₁₈ column and a water/methanol gradient. MS/MS transition (m/z) 313.3 鈫?241.2 was used for aflatoxin B₁ quantitation, with 313.3 鈫?285.1 used for confirmation. The limit of detection (LOD) for aflatoxin B₁ was 0.007 parts per billion (ppb). Method imprecision for aflatoxin B₁ (expressed as coefficient of variation) ranged from 5.5 to 9.4%. Spike recoveries were 105鈥?11%. Aflatoxin B₁ concentrations in the smokeless tobacco products analyzed ranged from <LOD to 0.271 ppb (dry mass). Aflatoxin B₁ was most frequently detected in dry snuffs and chews, whereas all moist snuff products tested were below LOD. The amounts of aflatoxin B₁ detected were low relative to the 20 ppb regulatory limit established by the U.S. Food and Drug Administration for foods and feeds.