分析测试学报2011,Vol.30Issue(1):6-12,7.DOI:10.3969/j.issn.1004-4957.2011.01.002
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
摘要
Abstract
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. 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≥O. 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-compontent mycotoxin contaminants in complex matrixes with advantages of simple pretreatment, good purification and high sensitivity.关键词
超高效液相色谱-串联质谱/凝胶渗透色谱/同位素内标/真菌毒素Key words
ultra performance liquid chromatography - tandem mass spectrometry ( UPLC - MS/MS)/ gel permeation chromatography (GPC)/ isotope internal standard/ myeotoxins分类
化学化工引用本文复制引用
宫小明,任一平,董静,孙军,李健,金超,于金玲..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[J].分析测试学报,2011,30(1):6-12,7.基金项目
山东检验检疫局科研基金资助项目(SK200822) (SK200822)