快速基质分散净化-超快速液相色谱-串联质谱法同时测定玉米中22种三嗪类除草剂残留  

Determination of 22 Triazine Herbicides Residual in Corn by Enhanced Matrix Removal Qu ECh ERS-Ultra Flow Liquid Chromatography-Tandem Mass Spectrometry

作　　者：吴岩[1,2] 赵伟 刘永 姜冰 魏冬旭 勾越 李丽丽[1] 韩峰[1] 祖元刚[1] 

机构地区：[1]东北林业大学森林植物生态学教育部重点实验室,哈尔滨150040 [2]黑龙江出入境检验检疫局,哈尔滨150001 [3]黑龙江省环境监测中心站,哈尔滨150056

出　　处：《分析化学》2016年第6期950-957,共8页Chinese Journal of Analytical Chemistry

基　　金：质检公益项目(No.201410177);黑龙江检验检疫局自主科研项目计划(No.2013HK002)资助

摘　　要：建立了玉米中扑灭津、莠去津、敌草净、特丁通等22种三嗪类除草剂多残留的分析方法。样品以乙腈为提取剂,经高速匀浆方法提取并浓缩后,以增强型脂质去除净化剂（EMR-Lipid）净化,除去了样品中的脂质,有效地降低了样品中的复杂基质所带来的背景干扰,净化液再经增强型脂质去除萃取剂（EMR-Polish）盐析萃取,以Kinetex XB-C_（18）柱为分离柱,用乙腈和0.1%甲酸溶液进行梯度洗脱,电喷雾正离子（ESI＋）多反应模式监测,超快度液相色谱-串联质谱（UFLC-MS/MS）测定,基质匹配标准曲线法定量。加标水平为5,10和20μg/kg时,22种农药的回收率为72%~105%,相对标准偏差小于15%。22种农药的检出限为0.16~1.8μg/kg,在1.0~50μg/L范围内线性关系良好（r〉0.993）。本方法具有快速、准确、灵敏度高等优点,能够准确测定玉米中22种三嗪类除草剂的残留量。An enhance matrix removal （ EMR） QuEChERS method for simultaneous determination of 22 triazine herbicide residuals such as atrazine, propazine, terbumeton, and desmetryn in corn was established and validated. The corn samples were initially extracted with acetonitrile （ MeCN ） in high-speed homogenization, and the targeted pesticides were prepared using EMR-Lipid （Enhanced matrix removal-lipid） method to clean-up and EMR-Polish to salt out, separated on a Kinetex XB-C18 with acetonitrile and 0. 1%formic acid aqueous as eluant, and then detected by UFLC-MS / MS under positive （ ESI＋ ） electrospray ionization and MRM models. The average recoveries of 22 herbicides were in the range of 72% -105% at the spiked level of 5, 10 and 20 μg / kg. The relative standard deviations were less than 15% . In the method validation, correlation coefficients were higher than 0. 993 with the linear range from 1. 0 μg / L to 50 μg / L. The qualitative analysis and quantitative analysis were investigated by UFLC-MS / MS and matrix-matched calibration curves. The results showed that EMR QuEChERS combined with UFLC-MS / MS purification method was rapid, accurate and sensitive for the determination of 22 triazine herbicides residues in corn.

关 键 词：脂质去除 快速基质分散净化 超快速液相色谱-串联质谱法 三嗪类除草剂 玉米 

分 类 号：O657.63[理学—分析化学]