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建立了芝麻酱中16种真菌毒素(赭曲霉毒素A、T-2毒素、伏马菌素B2、伏马菌素B1、O-甲基杂色曲霉素、蛇形菌素、新茄镰孢菌醇、杂色曲霉素、黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、曲酸、青霉酸、橘青霉素、黄曲霉毒素M1)多残留的超高效液相色谱-串联质谱(UPLCMS/MS)的检测方法。芝麻酱样品经乙腈-水-乙酸(80∶19∶1,体积分数,下同)溶液提取,QuEChERS方法净化后,以含0.1%甲酸的水溶液与乙腈为流动相,经ACQUITY UPLC BEH C18色谱柱(2.1mm×50mm,1.7μm)分离,以多级反应监测(MRM),外标法定量。结果表明:16种真菌毒素的检出限为0.03~1.5μg/kg,定量限为0.10~4.0μg/kg;线性范围在0.10~200μg/kg内各成分的线性相关系数均大于0.991;样品在定量限1倍、2倍和10倍3个添加水平下的平均回收率为70.7%~99.2%,相对标准偏差(RSD)为3.26%~10.5%。该方法简便、灵敏、快速,可用于芝麻酱中多种真菌毒素污染的监控分析。
Sixteen mycotoxins (ochratoxin A, T-2 toxin, fumonisin B2, fumonisin B1, O-methylascorbicans, sesbanin, Streptomyces albicans, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, kojic acid, penicillin, penicillin, aflatoxin M1) Phase chromatography - tandem mass spectrometry (UPLCMS / MS) detection method. The sesame samples were extracted with acetonitrile-water-acetic acid (80:19:1, the same below). After purifying by QuEChERS method, the mobile phase consisted of 0.1% formic acid in water and acetonitrile, and was analyzed by ACQUITY UPLC BEH C18 column 2.1mm × 50mm, 1.7μm) separation, multi-level reaction monitoring (MRM), external standard quantitative. The results showed that the detection limits of the 16 mycotoxins were 0.03-1.5 μg / kg and the limits of quantification were 0.10-4.0 μg / kg. The linear correlation coefficients of all the components in the range of 0.10-200 μg / kg were all greater than 0.991. The average recovery of 70% ~ 99.2% and RSD was 3.26% ~ 10.5% at the three loading levels of 1, 2 and 10 times of the limit of quantification. The method is simple, sensitive and rapid, and can be used for the monitoring and analysis of various mycotoxin contamination in sesame seeds.