超高效液相色谱串联质谱法测定花生、粮油中18种真菌毒素

Determination of 18 Mycotoxin Contaminants in Peanuts and Oils by Gel Permeation Chromatography and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

采用同位素稀释法并结合凝胶色谱净化技术，建立了花生、粮油中18种常见真菌毒素污染的超高效液相色谱串联质谱分析方法。样品中添加同位素内标U—[13C17]-黄曲霉毒素B1和U-[13C15]-脱氧雪腐镰刀菌烯醇，经乙腈-水溶液（84：16，体积比）均质提取，凝胶渗透色谱净化，WatersACQUITYUPLCTMBEHC18色谱柱分离，串联四极杆质谱多反应离子监测方式检测，同位素稀释内标法定量。结果表明，18种真菌毒素在各自的线性范围内线性关系良好，相关系数均不低于0．996；其中12种化合物的定量下限为0．02．0．4μg-kg，6种负离子的定量下限为0．06～1．0μg／kg；低、中、高3个加标水平的回收率为80％～96％，相对标准偏差为10．5％～19．6％。该方法具有前处理简单、净化效果好、灵敏度高的优点，适用于复杂基质样品中多组分真菌毒素残留的确认和定量检测。

A method for the analysis of common mycotoxins in peanuts and oils was developed using ultra performance liquid chromatography with tandem mass spectrometry（ UPLC -MS/MS）, based on isotope dilution and gel permeation chromatography （GPC） purification. The homogenized sample was spiked with U - [ 13C17 ] - aflatoxin B1 and U - [ 13C15 ] - deoxynivalenol）, and extracted with acetonitrile -water（84 ： 16, by volume）, then purified by GPC. The targeted compounds were detected by MS/MS system with eletrospray ionization（ESI） under muti-reaction monitoring（MRM） mode and quantified by the internal standard calibration curve of isotope dilution technique. The result indicated that the LOQ of 12 positive ions ranged from 0. 02μg/kg to 0.4μg/kg, the LOQ of 6 negative ions ranged from 0. 06μg/kg to 1.0 μg/kg. Meanwhile, the high correlation coefficents（r≥0. 996） of 18 mycotoxins were obtained within their respective linear ranges. The average recoveries at low, intermediate and high spiked levels ranged from 80% to 96% with relative standard deviations （RSD） of 10.. 5% - 19.6%. This method was suitable for the identification and quantification of multi-component mycotoxin contaminants in complex matrixes with advantages of simple pretreatment, good purification and high sensitivity.