气相色谱串联质谱法检测水产品中有机氯和菊酯农药残留  

Determination of Organochlorine and Chrysanthemum Ester Pesticides Residues in Aquatic Products Using Gel Permeation Chromatography and Gas Chromatography-Triple Quadrupole-Tandem Mass Spectrometry

作　　者：孟祥龙[1] 夏梦[1] 张云青[1] 范广宇[1] 徐文科[1] 唐秀[1] 段宏安[1] MENG Xiang-long;XIA Meng;ZHANG Yun-qing;FAN Guang-yu;XU Wen-ke;TANG Xiu;DUAN Hong-an(Lianyungang Entry-Exit Inspection and Quarantine Bureau, Lianyungang 222042, Jiangsu, China)

机构地区：[1]连云港出入境检验检疫局

出　　处：《食品研究与开发》2019年第16期153-158,共6页Food Research and Development

基　　金：江苏出入境检验检疫局项目(2017KJ12)

摘　　要：建立利用凝胶渗透色谱-气相色谱-三重四极杆串联质谱仪(gas chromatography-triple quadrupole-tandem mass spectrometry,GC-MS/MS)快速检测水产品中有机氯和菊酯类多种农药残留的方法,对样品提取溶剂进行优化,利用凝胶渗透色谱(gel permeation chromatography, GPC)结合分散固相萃取技术净化样品,并分别对农药化合物在GPC上的收集时间参数和N-丙基乙二胺(primary secondary amine,PSA)固相萃取吸附剂的添加量进行优化,在电子轰击电离源下进行多反应监测(multiple reaction monitoring,MRM)采集,该方法的检出限(limits of detection,LOD)为0.03 μg/kg^2.87 μg/kg,试验结果表明,该方法的回收率为60.5 %~118 %,相对标准偏差为0.75 %~15 %,该方法重现性好,精密度高,适用于泥鳅等水产品中有机氯和菊酯类农药残留的检测。A rapid method for the batch analysis of organochlorine and chrysanthemum ester pesticides in aquatic productions was established by gel permeation chromatography and gas chromatography-triple quadrupole-tandem mass spectrometry (GC-MS/MS),the extraction solvent of sample is optimized,GPC was employed to purify sample combined with dispersive solid-phase extraction (d-SPE), The optimal time for gathering samples were obtained as well as amount of PSA solid-phase extraction adsorbent for sample purification, detected by multiple reaction monitoring mode via electron impact ion source,the limits of detection of the pesticides in aquatic product was between 0.03 μg/kg-2.87 μg/kg,The experimental results showed that The average recoveries of pesticides varied from 60.5 % to 118 %,and the relative standard deviations were between 0.75 % and 15 %.The method had good reproducibility,high precision,therefore,it was suitable for the detection of a Multi-pesticide residues in loach and other aquatic products.

关 键 词：气相色谱串联质谱仪 凝胶渗透色谱 分散固相萃取 多农药残留 水产品 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]