QuEChERS-在线凝胶色谱-气相色谱-质谱法测定大米、黍子和小麦中34种农药残留

色谱 , 2013, 31(12): 1211-1217. doi: 10.3724/SP.J.1123.2013.07029

QuEChERS-在线凝胶色谱-气相色谱-质谱法测定大米、黍子和小麦中34种农药残留

阮华 ^1, , 荣维广 ^2, , 马永建 ^3, , 吉文亮 ^4, , 刘华良 ^5, , 宋宁慧 ^6,

1.东南大学公共卫生学院,江苏南京210009;江苏省疾病预防控制中心,江苏南京210009

2.江苏省疾病预防控制中心,江苏南京,210009

3.江苏省疾病预防控制中心,江苏南京,210009

4.江苏省疾病预防控制中心,江苏南京,210009

5.江苏省疾病预防控制中心,江苏南京,210009

6.环境保护部南京环境科学研究所,江苏南京,210042

基金项目: 江苏省疾病预防控制中心“科教兴业工程”项目(JKRC2011030) 国家自然科学基金项目(41101307) 江苏省“十二·五”科教兴卫工程项目(ZX201109)

关键词： QuEChERS , 凝胶色谱-气相色谱-质谱 , 农药残留 , 快速筛查

Determination of 34 pesticide residues in rice, proso millet and wheat with QuEChERS-on line gel permeation chromatography-gas chromatography-mass spectrometry

Keywords： QuEChERS , gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS) , pesticide residues , fast screening

采用QuEChERS方法结合在线凝胶色谱-气相色谱-质谱(GPC-GC-MS)系统,建立了大米、黍子和小麦中34种中高毒农药的快速筛查方法.研究了称样量、萃取剂、净化吸附剂种类对大米样品提取净化效果的影响并考察了基质效应和分析保护剂的使用效果,采用选择离子监测(SIM)模式,外标法定量.结果表明,34种农药在大米、黍子和小麦中的检出限分别为0.028 1 ～5.30、0.0282～4.82、0.027 3～5.13 μg/kg;在0.05 μg/g添加水平的平均回收率分别为94.5％～ 117.1％、83.1％～ 121.7％、93.1％～ 120.2％;相对标准偏差(RSD,n=6)分别为2.6％～14.5％、3.4％～15.1％、3.5％～ 15.2％.该方法消耗试剂少,分析成本低,符合绿色化学的理念,具有操作便捷、快速、通用性强等特点,适用于大米、黍子和小麦中34种农药残留的快速筛查与检测.

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