快速样品前处理技术-超高效液相色谱串联质谱法测定粮谷中7种真菌毒素

Determination of seven mycotoxins ingrains using QuEChERS andultra-performance liquid chromatography-tandem mass spectrometry

QuEChER是一种快速样品前处理技术(quick、easy、cheap、effective、rugged和safe, QuEChER),本文构建QuEChERS-超高效液相色谱串联质谱(UPLC-MS/MS)法检测粮谷中7种真菌毒素残留的方法。样品经过乙腈-水-甲酸(体积比为84?15.5?0.5)溶液提取,提取液采用N-丙基乙二胺(PSA)净化,UPLC-MS/MS法分析检测。结果表明:质量浓度为0.15~250μg/L时,7种真菌毒素线性关系良好,相关系数(R~2)大于0.99,方法检出限为0.02~13.22μg/L,定量限为0.08~39.55μg/L,小麦中7种毒素平均加标回收率为82.44%~103.12%,RSD小于10%;利用该方法检测大米、豆类和花生等多种粮谷作物中7种真菌毒素的加标回收率均大于82%。该方法简单快速、灵敏度和准确度高,能满足粮谷中7种毒素的分析。

QuEChER,a fast and fast sample preprocessing technology(quick、easy、cheap、effective、rugged、safe),was applied to determine the contents of seven mycotoxin residues in grains through the combination with UPLC-MS/MS.After the samples were extracted with acetonitrile-water-formic acid(84∶15.5∶0.5)solution and purified by N-propyl ethylene diamine(PSA),UPLC-MS/MS was used for the detection.The excellent linearity was observed for the seven mycotoxins in the concentration range of 0.15-250μg/L,with the correlation coefficients(R 2)higher than 0.99.In addition,the detection and quantification limits of our method were 0.02-13.22μg/L and 0.08-39.55μg/L,respectively.The average spiked recoveries were 82.44%-103.12%,with RSD less than 10%.When this method was utilized to measure the seven mycotoxins in rice,beans,peanuts and other cereal crops,the spiked recoveries turned out to be greater than 82%,further demonstrating the general applicability of our analytical method.