利用免疫亲和萃取结合超高效液相色谱-串联四极杆质谱技术（UPLC-MS/MS）建立了乳及乳制品中黄曲霉毒素M1和M2的提取、分离、确证与定量方法。乙腈和水提取样品中的黄曲霉毒素，乙腈二次去蛋白后用免疫亲和柱净化，采用Waters Acquity UPLC R HSS T3（2.1×100 mm，1.7μm）色谱柱实现分离，多反应监测（MRM）模式下以外标法定量。结果表明：黄曲霉毒素M1和M2在0.1μg/L~50μg/L范围内线性关系良好（r﹥0.9985）；检出限为0.029μg/L~0.047μg/L（S/N=3）；2种黄曲霉毒素各添加水平在鲜牛奶、奶粉和奶油中的回收率为在69.56%~88.43%之间；相对标准偏差为3.69%~8.74%。%A method for the determination of 2 aflatoxins (M1,M2) in milk and dairy products by immunoaffinity extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/M S) was developed. Aflatoxins in samples were extracted into acetonitrile/water system and deproteinized by adding additional acetonitrile, followed by stepwise purification using an immunoaffinity column. The target compounds were then eluted with methanol. With the gradient elution using a binary mobile phase containing of 0.1%formic acid solution and methanol/acetonitrile, the two aflatoxins were separated on a Waters Acquity UPLC R HSS T3 column (2.1 ×100 mm,1.7 μm particle size), followed by positive electrospray ionization and multi reaction monitoring provided by a triple-quadrupole tandem mass spectrometer,and quantified by external reference method. The calibration curve was linear over the concentration range of 0.1μg/L-50μg/L (r﹥0.998 5) and the detection limits of two aflatoxins were 0.029μg/L-0.047μg/L. The recoveries from milk, milk powder and cream were generally between 69.56%and 88.43%and the relative standard deviations were 3.69%-8.74%.
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