凝胶渗透色谱-气相色谱-串联质谱法测定蔬菜水果中41种农药残留  

Determination of 41 pesticides in vegetables and fruits by GPC-GC-MS/MS

作　　者：封利会[1] 王硕[1] 张向明[1] 毛红霞[1] 

机构地区：[1]北京市朝阳区疾病预防控制中心,北京100021

出　　处：《卫生研究》2016年第1期68-75,共8页Journal of Hygiene Research

摘　　要：目的通过比较不同的提取溶剂和提取净化方法，建立了QuEChERS前处理，在线凝胶色谱-气相色谱-串联质谱法（GPC—GC—MS／MS）快速测定蔬菜水果中41种农药的检测方法。方法样品经乙腈-乙酸乙酸钠缓冲液均质提取，混合型固相分散萃取剂净化，凝胶渗透色谱气相色谱串联质谱，MRM模式检测。结果在2～200ng／mL范围内，41种农药的线性相关系数均大于0．995，在芹菜和苹果两种样品基质中添加41种农药，添加水平为5、10和50μg／kg的混合标准溶液，41种农药的平均回收率范围为71．0％～125．4％，相对标准偏差范围为0．34％～15．00％。添加水平为5μg／kg时的定量限为0．107～10．100μg／kg。结论该方法样品处理简单快速，相比其他多残留分析方法净化效果好，其灵敏度和选择性明显提高。Objective A method for the determination of 41 pesticides including 26 organophosphorus pesticides, 6 kinds of carbamate, 7 pryethoids insecticides, 1 kinds of organochlorine and fungicide in vegetables and fruits,was established based on optimized QuEChERS with on line gel permeation chromatography-gas chromatography-mass spectrometry （GPC-GC-MS/MS）. Methods The method obtained the optimized conditions by comparing different methods of extraction and purification. The analytes were extracted from the samples using acetonitrile-buffer of acetic acid and sodium acetate. Then the extracts were determined by GC-MS/MS in muhireaction monitoring（MRM） mode after being cleaned up with mixed solid-phase dispersion. And the external standard method was applied to quantify. Results All the 41 pesticides had good linearity in the ranges of 2 - 200 ng/mL with the correlation coefficients higher than 0. 995. The average recoveries of the most of 41 pesticides in celery and apple were in the range of71.0%-125.4% at the spiked levels of 5, 10 and 50 μg/kg,with relative standard deviations（RSDs） of 0.34%- 15.0% . The limits of quantification（LOQs） of the method at the spiked levels of 5 μg/kg were 0. 107 - 10. 100 μg/kg. Conclusion The method is simple, rapid, sensitive and specific.

关 键 词：农药残留 凝胶渗透色谱一气相色谱.串联质谱 QuEChERS法 蔬菜 水果 

分 类 号：R155.54[医药卫生—营养与食品卫生学] TS207.53[医药卫生—公共卫生与预防医学]