QuEChERS法结合在线凝胶色谱-气相色谱/质谱法测定人体尿液中34种农药残留  

Determination of 34 pesticides in urine with QuEChERS-on line gel permeation chromatography-gas chromatography/mass spectrometry

作　　者：荣维广[1] 阮华 吴建[1] 马永建[1] 吉文亮[1] 刘华良[1] 宋宁慧[3] 

机构地区：[1]江苏省疾病预防控制中心,江苏南京210009 [2]江苏辉丰农化股份有限公司,江苏盐城224100 [3]环境保护部南京环境科学研究所,江苏南京210042

出　　处：《中国食品卫生杂志》2015年第3期253-257,共5页Chinese Journal of Food Hygiene

基　　金：国家自然科学基金(41101307);江苏省科技厅科技支撑计划项目(BE2010745);江苏省疾病预防控制中心"科教兴业工程"项目(JKRC2011030)

摘　　要：目的建立Qu ECh ERS方法结合在线凝胶渗透色谱-气相色谱/质谱系统用于人尿中34种中高毒农药的快速筛查方法。方法研究Qu ECh ERS各因素如萃取剂、萃取剂用量、萃取次数和净化吸附剂种类对尿样提取净化效果的影响。采用选择离子监测模式,外标法测定人尿中34种农药含量。结果 34种农药在人尿中的检出限为0.05~3.2μg/kg,在0.05μg/g添加水平的平均回收率为81.1%~108.8%,相对标准偏差（RSD）为2.7%~10.4%。结论本法具有操作便捷、通用性强等特点,适用于人尿中34种农药残留的快速筛查与检测。Objective A method for the simultaneous determination of 34 pesticides in urine by QuEChERS coupled with on line gel permeation chromatography-gas chromatography-mass spectrometry （GPC-GC/MS） was developed. Methods The effect of extraction and purification which the extraction and combinations of sorbent involved were investigated. The identification and quantification were performed by GPC-GC/MS in SIM mode and external standard method. Results The LOD of this method ranged from O. 05-3.2 μg/kg （S/N = 3） in urine, the average recoveries of 34 pesticides for samples spiked at 0. 05 μg/g ranged from 81. 1% -108.8% with the relative standard deviations （RSD, n =6） less than 10.4%. Conclusion The convenient operation and versatility of this method is suitable for the fast screening and detection of 34 pesticide residues in urine.

关 键 词：QU ECh ERS 凝胶色谱-气相色谱/质谱 尿液 农药残留 快速筛查 

分 类 号：R446.12[医药卫生—诊断学]