分散固相萃取-气相色谱-质谱法测定牛奶中多组分农药残留  

Determination of multicomponent pesticide residues in milk by dispersive-SPE and GC-MS

作　　者：侯逸众[1] 黄方取 胡浩军[1] 严继东[1] 申屠平平[1] 徐小民[2] 

机构地区：[1]金华市疾病预防控制中心,浙江金华321002 [2]浙江省疾病预防控制中心,浙江杭州310051

出　　处：《中国卫生检验杂志》2016年第16期2291-2295,共5页Chinese Journal of Health Laboratory Technology

基　　金：浙江金华市科技局资助项目(2014-3-102)

摘　　要：目的建立内标稀释-分散固相萃取-气相色谱-质谱法测定牛奶中有机磷、有机氯、菊酯类等多组分农药残留方法,为牛奶中农药残留检测提供参考。方法样品加入乙腈、无水硫酸镁、氯化钠提取后,取上层有机相清液加入C18、PSA和无水硫酸镁作为分散固相萃取试剂去除杂质,浓缩后用气相色谱-质谱仪测定,配制基质标准曲线采用内标法定量。结果 57种农药组分在考察范围内保持良好的线性关系,相关系数为0.995 3-0.999 9,加标回收率为58.7%-127.1%,相对标准偏差（RSD）为0.5%-6.8%（n=6）。结论该方法操作方便,试剂消耗量少,回收率稳定,结果准确可靠,适合快速筛查牛奶中有机磷、有机氯、菊酯类等多组分农药残留。Objective To establish a method for the determination of multi-component pesticide residues such as organophosphate,organochlorine,pyrethroids by internal standard dilution-dispersive SPE-gas chromatography-mass spectrometry,so as to provide reference for the detection of pesticide residues in milk.Methods Sample was extracted by acetonitrile,anhydrous magnesium sulfate and sodium chloride.The supernatants were purified by dispersive solid phase extraction using C18,PSA and anhydrous magnesium sulfate as dispersing agents,analyzed by GC-MS after concentration.The matrix-matched internal standard calibration curves were used for quantitative analysis.Results Good linearity was obtained when the concentrations of these pesticides were within the corresponded range,with the correlation coefficient within 0.995 3-0.999 9,the spiked recoveries within 58.7%-127.1%,and the relative standard deviation（RSD） of 0.5%-6.8%（n=6）.Conclusion The method is easy to operate,accurate and reliable with less reagent consumption and stable recoveries,which is suitable for the rapid screening of multi-component pesticide residues such as organophosphate,organochlorine,pyrethroids in milk.

关 键 词：分散固相萃取 气相色谱-质谱法 牛奶 农药 

分 类 号：O657.63[理学—分析化学]