[1]高尧华,滕爽,宋卫得,等.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,2018,37(02):284-294.[doi:10.11861/j.issn.1000-9841.2018.02.0284]
　GAO Yao-hua,TENG Shuang,SONG Wei-de,et al.Detection Methods of 56 Pesticide Residues in Soybean, Peanut and Grain Oil[J].Soybean Science,2018,37(02):284-294.[doi:10.11861/j.issn.1000-9841.2018.02.0284]
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大豆、花生及粮油中56种农药残留量的检测方法

《大豆科学》[ISSN:1000-9841/CN:23-1227/S] 卷: 第37卷 期数: 2018年02期 页码: 284-294 栏目: 出版日期: 2018-03-20
Title:
Detection Methods of 56 Pesticide Residues in Soybean, Peanut and Grain Oil
作者:
高尧华1; 滕爽2; 宋卫得1; 刘冰1
（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）
Author(s):
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, China)
关键词:
气相色谱/串联三重四级杆质谱; 粮油; 农药残留
Keywords:
Gas chromatography/triple quadrupole mass spectrometry;  Grain oil;  Pesticide residues
分类号:
O657.63
DOI:
10.11861/j.issn.1000-9841.2018.02.0284
文献标志码:
A
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。
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.

参考文献/References:

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备注/Memo

收稿日期：2017-12-11

基金项目：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）。
第一作者简介：高尧华（1982-），女，硕士，工程师，主要从事食品检测研究。 E-mail:gaoyaohua123@163.com。
通讯作者：宋卫得（1981-），男，硕士，高级工程师, 主要从事食品检测研究。E-mail:woxinyh2006@163.com。

更新日期/Last Update: 2018-04-02