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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

宫小明 任一平 董静 孙军 李健 金超 于金玲

分析测试学报2011,Vol.30Issue(1):6-12,7.
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

宫小明 1任一平 2董静 1孙军 1李健 3金超 1于金玲1

作者信息

  • 1. 潍坊出入境检验检疫局,山东,潍坊,261041
  • 2. 浙江省疾病预防控制中心,浙江,杭州,310051
  • 3. 中国水产科学研究院黄海水产研究所,山东,青岛,266071
  • 折叠

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)

分析测试学报

OA北大核心CSCDCSTPCD

1004-4957

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