GPC-UPLC-MS/MS法测定植物油中的黄曲霉毒素

Determination of Aflatoxins in Vegetable Oil by GPC-UPLC-MS/MS

建立了凝胶色谱净化-超高效液相色谱-串联质谱联用测定植物油中四种黄曲霉毒素B1、B2、G1、G2含量的分析方法。该方法用乙酸乙酯-环己烷(1︰1, V/V)提取植物油样品,加入黄曲霉毒素同位素内标物后经凝胶色谱净化及在线浓缩,以0.1%甲酸水溶液-乙腈作为流动相梯度洗脱,采用C18色谱柱(50 mm×2.1 mm, 1.8μm),在电喷雾离子源ESI正离子模式下以多重反应监测(MRM)测定。结果表明, 4种黄曲霉毒素在0.2~10 ng/mL的范围内与峰面积有良好的线性关系,相关系数大于0.99,检出限为0.037~0.086μg/kg,加标回收率在92.9%~108.2%之间,相对标准偏差(RSD)为3.6%~8.2%。该方法简便灵敏、准确快速、重现性好、自动化程度高、杂质干扰少,适用于植物油等食品中黄曲霉毒素的测定。

A determination method of four aflatoxins(B1, B2, G1 and G2) in vegetable oil was established by gel permeation chromatography(GPC)-ultra performance liquid chomatography-tandem mass spectrometry(UPLC-MS/MS). The samples added isotope internal standard substances were extracted by ethyl acetate/cyclohexane(1︰1, V/V), then purified by GPC and on-line concentrated. The target compound was separated by Agilent ZORBAX SB-C18 column(50 mm×2.1 mm, 1.8 μm) using 0.1% formic acid water-acetonitrile as mobile phase and analyzed by electrospray ionization(ESI) in the positive ion and multiple reaction monitoring mode(MRM). The results show that the range of four aflatoxins from 0.2 to 10 ng/mL had good linear relationship with the peak area;The quantitative limits were 0.037-0.086 μg/kg;The average recoveries for them were between 92.9% and 108.2%;The RSDs were between 3.6% and 8.2%. The method is simple, accurate, rapid, reproducible, highly automated and less interference. It is suitable for the determination of aflatoxins in vegetable oil and other foods.