市售调味酱中5种真菌毒素的测定

Determination of Five Mycotoxins in Commercially Available Seasoning Sauce

建立了用超高效液相色谱-串联质谱同时检测芝麻酱、花生酱及黄豆酱中5种真菌毒素(黄曲霉毒素B_(1)、黄曲霉毒素B_(2)、黄曲霉毒素G_(1)、黄曲霉毒素G_(2)、赭曲霉毒素A)的检测方法。样品采取乙腈-甲酸-水(70∶1∶29,体积比)混合溶液提取,利用多功能净化柱净化,采用1%的甲酸水相和混合甲醇-乙腈有机相进行梯度洗脱,经多反应监测模式测定样品中的目标化合物,采用内标法定量。5种真菌毒素在浓度0.10~100.0μg/L范围内具有良好的线性关系,相关系数均大于0.999,样品测定的方法检出限为0.05~0.20μg/kg,定量限为0.20~0.70μg/kg,3个添加浓度水平的平均回收率为87.1%~103.4%,相对标准偏差为1.18%~5.26%。该方法灵敏度高、操作便捷、快速准确,可适用于多种调味酱中5种真菌毒素的污染监测情况分析。

A method is established for the simultaneous determination of five mycotoxins such as aflatoxin B_(1),aflatoxin B_(2),aflatoxin G_(1),aflatoxin G_(2) and ochratoxin A in sesame paste,peanut paste and soybean paste by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples are extracted with the mixed solution of acetonitrile-formic acid-water(70∶1∶29,volume ratio)and purified with multi-functional purification column,the aqueous phase of 1%formic acid and organic phase of mixed methanol-acetonitrile are used for gradient elution.The target compounds in the samples are determined by multi-reaction monitoring mode and quantified by internal standard method.The five mycotoxins show good linear relationship in the concentration range of 0.10~100.0μg/L,and the correlation coefficients are all greater than 0.999.The detection limits and quantification limits of the determination method are 0.05~0.20μg/kg and 0.20~0.70μg/kg respectively.The average recovery rates of the three additive levels are 87.1%~103.4%with relative standard deviations(RSDs)of 1.18%~5.26%.The method has high sensitivity,convenient operation and is rapid and accurate,which can be used to monitor the contamination of five mycotoxins in various seasoning sauces.