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

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,Waters ACQUITY UPLCTM ...

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

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——aflatoxin B1 and U——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 0.02 μg/kg to 0.4 μg/kg,the LOQ of 6 negative ions ranged from 0.06 μg/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.