Determination of Aflatoxin B-1 in Smokeless Tobacco Products by Use of UHPLC-MS/MS

摘要

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 B-1 concentrations in 32 smokeless tobacco products commercially available in the United States. Smokeless tobacco products were dried, milled, and amended with C-13(17)-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 B-1, B-2, G(1), and G(2) in a 2.5 min run by use of a fused core C-18 column and a water/methanol gradient. MS/MS transition (m/z) 313.3 -> 241.2 was used for aflatoxin B-1 quantitation, with 313.3 -> 285.1 used for confirmation. The limit of detection (LOD) for aflatoxin B-1 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 105-111%. Aflatoxin B-1, concentrations in the smokeless tobacco products analyzed ranged from