大豆、花生及粮油中56种农药残留量的检测方法  

Detection Methods of 56 Pesticide Residues in Soybean,Peanut and Grain Oil

作　　者：高尧华 滕爽[2] 宋卫得 刘冰 GAO Yao-hua1, TENG Shuang2 , SONG Wei-de1 , LIU Bing1(1. Rizhao Entry-Exit Inspection and Quarantine Bureau, Rizhao 276826, China; 2. Nanjing Agricultural University, Nanjing 210095, Chin)

机构地区：[1]日照出入境检验检疫局,山东日照276826 [2]南京农业大学,江苏南京210095

出　　处：《大豆科学》2018年第2期284-294,共11页Soybean Science

基　　金：国家质量监督检验检疫总局科技项目(2016IK206);山东检验检疫局科技项目(SK201761;SK201619)

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。In order to study the pesticide residues in the source samples of grain and grain oil, a muhiresidue analytical meth- od for the rapid determination of 56 pesticide residues in soybean, peanut and grain oil was established by gas chromatogra- phy/triple quadrupole mass spectrometry（GC/MS/MS）. The MS/MS detection paramete/s and presample treatment were opti- mized. 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-l , 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.

关 键 词：气相色谱/串联三重四级杆质谱 粮油 农药残留 

分 类 号：O657.63[理学—分析化学]