固相萃取-高效液相色谱/串联质谱检测谷物中黄曲霉毒素B_1、B_2、G_1、G_2和M_1

Determination of aflatoxin B_1,B_2,G_1,G_2 and M_1 in corn by high performance liquid chromatography-tandem mass spectrometry

建立了高效液相色谱/串联质谱(LC-MS/MS)同时检测谷物中的黄曲霉毒素B1、B2、G1、G2和M1的方法。并优化了液相色谱条件和质谱的相关参数。谷物样品经研磨成粉末后,直接经甲醇-水(V:V=10:90)提取,Oasis HLB固相萃取净化,乙腈-水(0.2%甲酸)梯度洗脱,选择电喷雾离子源(ESI),正离子扫描多反应监测(MRM)模式,外标法定量。黄曲霉毒素B1、B2、G1、G2和M1的定量下限分别为0.1、0.1、0.2、0.3、0.2 ng/g,平均回收率在74.6%～89.6%之间,测试精密度(RSD)在5.2%～11.3%之间。方法已用于谷物样品检测,黄曲霉毒素残留量最高达到B1 5.86 ng/g、G1 8.6 ng/g、M1 4.0 ng/g,B2和G2未检出。

A sensitive method was developed for the determination of aflatoxin B1,B2,G1,G2 and M1 in corn by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.Analysis conditions of liquid chromatography and mass spectrometry were optimized.Aflatoxins were extracted with 10%（V/V） methanol-water after corn was grinded into powder,purified through an Oasis HLB cartridge,eluted by methanol and water containing 0.2% formic acid,and determinated by electrospray ionization in positive ion mode and using multiple reaction monitoring（MRM）.The limits of quantification for aflatoxin B1,B2,G1,G2 and M1 were 0.1 ng/g,0.1 ng/g,0.2 ng/g,0.3 ng/g and 0.2 ng/g,the correlation coefficients were more than 0.9975 in respective linear ranges,and recoveries for analytes in different matrixs were 74.6% ~ 89.6% and the relative standard deviations（RSD） in different concentration levels were all less than 11.3%.The proposed method was sensitive to meet the requirements for monitoring aflatoxin B1,B2,G1,G2 and M1 in corn.