同位素稀释气相色谱-串联质谱法测定乳制品中27种有机氯农药及代谢物  

Determination of organochlorine pesticides and their metabolites in dairy products by isotope dilution gas chromatography-tandem mass spectrometry

作　　者：倪蓉[1] 陈翔[1] 卢大胜[2] 汪国权[2] NI Rong;CHEN Xiang;LU Da-sheng;WANG Guo-quan(Xuhui District Center for Disease Control and Prevention,Shanghai 200237,China)

机构地区：[1]上海市徐汇区疾病预防控制中心,上海200237 [2]上海市疾病预防控制中心,上海200336

出　　处：《中国卫生检验杂志》2019年第1期8-12,共5页Chinese Journal of Health Laboratory Technology

基　　金：上海市徐汇区医学科研项目(SHXH201408)

摘　　要：目的建立乳制品中27种持久性有机氯农药及代谢物的同位素稀释气相色谱-串联质谱法。方法样品经过加速溶剂萃取提取后,经过凝胶色谱和固相萃取联合净化,采用气相色谱-串联质谱法测定,同位素稀释内标法定量。结果在0. 5 ng/ml～200 ng/ml的线性范围内,27种物质的线性关系良好,相关系数均> 0. 998;方法的最低检测浓度为0. 07 ng/kg～1. 7 ng/kg;在0. 016μg/kg、0. 080μg/kg高、低2个水平的加标浓度下,空白基质奶粉的平均回收率为70. 5%～118. 8%,相对标准偏差为2. 1%～14. 4%。用所建方法对20份市售乳制品进行了测定,结果满意。结论该方法灵敏度和准确度高,选择性好,适用于乳制品中有机氯农药及代谢物的测定。Objective To develop a method for the determination of 27organochlorine pesticides and their metabolites(OCPs) in dairy products by isotope dilution gas chromatography-tandem mass spectrometry (ID-GC -MS/MS).Methods The samples were initially extracted by accelerated solvent extraction (ASE ),followed by cleaning -up using gel chromatography (GPC)and solid phase extraction(SPE),finally determined by GC -MS/MS.The quantification was based on the isotope dilution internal standard method.Results Good linearity was obtained when the concentrations of the 27organochlorine pesticides were within 0.5ng,/ml -100ng/ml,with the correlative coefficients greater than 0.998.The lowest detection limit was within 0.07ng/kg -1.7ng/kg.The average recoveries of blank matrix milk powder spiked at two levels were within 70.5%-118.8%,with the relative standard deviations(RSDs)within 2.1%-14.4%.The established method was applied in determining the 27 OCPs in 20dairy products,and the results were satisfactory.Conclusion This method is sensitive and accurate, and suitable for the determination of organochlorine pesticides and metaholites in dairy products.

关 键 词：同位素稀释气相色谱一串联质谱 乳制品 有机氯农药及代谢物 

分 类 号：O657.63[理学—分析化学]