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大豆、花生及粮油中56种农药残留量的检测方法
引用本文:高尧华,滕爽,宋卫得,刘冰.大豆、花生及粮油中56种农药残留量的检测方法[J].大豆科学,2018(2):284-294.
作者姓名:高尧华  滕爽  宋卫得  刘冰
作者单位:日照出入境检验检疫局,山东日照,276826 南京农业大学,江苏南京,210095
基金项目:国家质量监督检验检疫总局科技项目,山东检验检疫局科技项目
摘    要:为研究高油脂植物源性样品粮谷和粮油中的农药残留量,本研究建立了气相色谱/串联三重四级杆质谱法(GC/MS/MS)能够快速、简单、同时测定大豆、花生及其粮油中56种农药残留,并对MS/MS检测参数及样品前处理方式进行了优化。样品经乙腈提取后,冷冻、离心,串联C18/PSA固相萃取柱净化,采用气相色谱/串联三重四级杆质谱仪检测,56种农药在线性范围内均呈现良好的线性关系,线性系数大于0.99。本检测方法的检出限(LOD)为0.001~0.005 mg·kg~(-1),方法验证试验结果表明,该类化合物的平均回收率为62%~116%,相对标准偏差(RSD)为0.82%~14.5%。本方法重现性好,精密度高,操作简单,适用于大豆、花生及其粮油类高油脂植物源性食品中多种农药残留的检测。

关 键 词:气相色谱/串联三重四级杆质谱  粮油  农药残留  Gas  chromatography/triple  quadrupole  mass  spectrometry  Grain  oil  Pesticide  residues

Detection Methods of 56 Pesticide Residues in Soybean,Peanut and Grain Oil
GAO Yao-hua,TENG Shuang,SONG Wei-de,LIU Bing.Detection Methods of 56 Pesticide Residues in Soybean,Peanut and Grain Oil[J].Soybean Science,2018(2):284-294.
Authors:GAO Yao-hua  TENG Shuang  SONG Wei-de  LIU Bing
Abstract:In order to study the pesticide residues in the source samples of grain and grain oil,a multiresidue analytical method for the rapid determination of 56 pesticide residues in soybean,peanut and grain oil was established by gas chromatography/triple quadrupole mass spectrometry(GC/MS/MS).The MS/MS detection parameters and presample treatment were optimized.The samples were extracted by acetonitrile,freezing,centrifuge,and purification treatment by series C18/PSA solid phase extraction column and detected by gas chromatography/triple quadrupole mass spectrometry (GC/MS/MS).The 56 pesticides in linear range showed good linear relationship,the linear coefficient was greater than 0.99.The detection limit (LOD) was 0.001-0.005 mg·kg-1,the validation test results showed that the recovery of the compounds was between 62% -116% and relative deviation (RSD) was between 0.82%-14.5%.The method has good reproducibility,high precision and simplicity suitable for a variety of pesticide residues detection as soybean,peanut,grain oil and most plant sources.
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