UPLC-MS/MS测定乳制品中伏马毒素B1、B2残留

Determination of Fumonisin B1, B2 in Dairy Products by UPLC-MS/MS

为建立一种UPLC-MS/MS测定乳制品中伏马毒素B1、B2残留的检测方法,乳制品经过溶解后以氢氧化钠溶液调节pH至弱碱性,用PBS缓冲液进行稀释,再用伏马毒素免疫亲和柱进行净化。0.1%甲酸水溶液-乙腈作为流动相,采用C18色谱柱,再用UPLC-MS/MS进行定性、定量测定,外标法定量。结果表明:伏马毒素B1、B2线性关系良好,相关系数均大于0.99,线性范围为0.5~50μg/L,样品在1.0~10μg/kg加标浓度下回收率为80.3%~96.7%,变异系数为2.3%~8.8%,检出限为0.5μg/kg,定量限为1.0μg/kg。该方法能够准确、稳定、灵敏地测定乳制品中伏马毒素的残留。

A detection method was developed for fumonisin B1, B2 residues in dairy products by liquid chromatographytandem mass spectrometry. After the dairy products were dissolved, samples’ pH was adjusted to weak alkalinity by NaOH solution, then diluted with PBS buffer and purified by immunoaffinity column. 0.1% Formic acid aqueous solution-acetonitrile was used as mobile phase. The analyses were performed on a C18 column with 0.1% formic acid aqueous solution-acetonitrile as the mobile phase. The test was determined by liquid chromatography-tandem mass spectrometry. The results showed that fumonisin B1 and B2 had good linear relationships. The correlation coefficients were greater than 0.99. The recoveries of fumonisin B1 and B2 were 80.3 and 96.7%, the coefficients of variation were 2.3 and 8.8%, the detection limit was 0.5 μg/kg, and the quantitative limit was 1.0 μg/kg. This method could be accurate, stable, sensitive for the determination of Fumonisin residues in dairy products.