QuEChERS/HPLC-MS/MS法同时测定果蔬中17种农药残留
Determination of 17 Pesticide Residues in Fruits and Vegetables by QuEChERS Method Coupled with High Performance Liquid Chromatography Tandem Mass Spectrometry
郭保宝 1石志格 2刘胜男 3张国庆 1韩四海4
作者信息
- 1. 三门峡市检验检疫中心,河南三门峡472000
- 2. 三门峡市检验检疫中心,河南三门峡472000;三门峡出入境检验检疫局,河南三门峡472000
- 3. 三门峡出入境检验检疫局,河南三门峡472000
- 4. 河南科技大学食品与生物工程学院,河南洛阳471023
- 折叠
摘要
[目的]利用高效液相色谱-串联质谱(HPLC-MS/MS)检测技术,建立了果蔬中同时测定17种农药残留的分析方法.[方法]采用QuEChERS前处理方法,用含1％(V/V)乙酸的乙腈溶液提取样品,以无水硫酸镁(MgSO4)作为脱水剂,经N-丙基乙二胺(PSA)和石墨化碳黑(GCB)混合净化剂净化,C18色谱柱分离,高分辨质谱在正离子模式下选用多重反应监测(MRM)扫描测定,基质匹配标准曲线外标法定量.[结果]17种农药在1～50 ng/mL范围内线性关系良好,相关系数均在0.99以上.分别对黄瓜、苹果进行3个加标水平的回收试验(1.0、2.0、5.0μg/kg),17种目标物的回收率为60.2％ ～117.7％,相对标准偏差低于12.8％.检出限(S/N≥3)为0.2μg/kg,定量限(S/N≥10)为1.0μg/kg.[结论]该方法简单、快速、灵敏、精确,能够同时准确测定果蔬样品中17种农药残留.
Abstract
[ Objective] A rapid and effective method was established for the simultaneous determination of 17 pesticide residues in fruits and vegetables by high performance liquid chromatography tandem mass (HPLC-MS/MS). [Method] Using modified QuEChERS method, the samples was extracted with acetonitrile containing 1％ ( V/V) acetic acid, purified by a mixed sorbent of MgSO4 , primary secondary amine ( PSA) and graphitized carbon black ( GCB) , separated on a C18 column and analyzed by postitive electrospray ionization tandomd method. [ Result] The results showed that the 17 pesticide residues were linear in the range of 1-50 ng/mL with correlation mass spectrometry under multiple reactions monitoring (MRM) mode. The quantitative analysis was used by external standarcoefficients(r) over 0. 99. The recoveries at spiked levels of 1. 0 , 2. 0 and 5. 0 μg/kg for all target compounds in the samples were in the range of 60. 2％ -117. 7％, with relative standard deviations less than 12. 8％. The limits of detection (LOD, S/N≥3) was 0. 2 μg/kg;the limits of quantitation (LOQ, S/N≥10) was 1. 0 μg/kg. [Conclusion] A simple, rapid, sensitive and accurate method was developed, which was suitable for the determination of 17 pesticide residues in fruits and vegetables simultaneously.
关键词
QuEChERS/高效液相色谱-串联质谱/同时测定/果蔬/农药残留Key words
QuEChERS/High performance liquid chromatography tandem mass/Simultaneous determination/Fruits and vegetables/Pesticide residues引用本文复制引用
基金项目
河南省科技攻关计划项目(152102110025)
出版年
2017
国家科技期刊平台
NSTL
维普
万方数据