凝胶渗透色谱和固相萃取净化气相色谱-质谱法检测动物性食品中26种有机氯农药残留  

Determination of 26 organochlorine pesticides residues in animal food by gas chromatography/mass spectrometry with purification of gel permeation chromatography and solid phase extraction

作　　者：曹忠波[1] 高岩[1] 贾宏新[1] 

机构地区：[1]辽宁省疾病预防控制中心,沈阳110005

出　　处：《中国卫生检验杂志》2012年第7期1550-1552,1554,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的:建立一种测定动物性食品中有机氯类多种农药残留的气相色谱质谱分析方法。方法:采用丙酮和正己烷提取肉中多种有机氯类农药,以凝胶渗透色谱(GPC)和固相萃取(SPE)净化、浓缩后,用气相色谱—质谱选择离子监测方式分析检测26种有机氯农药残留。结果:所有26种农药均在20 min内流出,分离良好,农药标准的线性范围在0.01 mg/L～0.5 mg/L相关系数r均在0.99以上,低、高两种浓度加标回收率均在61%～95%之间,相对标准偏差均小于13%,方法最低检出限在0.002 mg/kg～0.005 mg/kg。结论:本方法适合动物性食品中有机氯类农药残留的测定。Objective：To establish a method for determination of organochlorine pesticide in animal food by gas chromatography/mass spectrometry（GC/MS） and selected ion monitoring（SIM）.Methods： The pesticides were extracted with acetone and hexanes.The extract was cleaned-up by gel permeation chromatography and solid phase extraction.The analysis was performed by gas chromatography/mass spectrometry（GC/MS） and selected ion monitoring（SIM）.Retention time and ion abundance ratio were used to confirm the pesticides.Results： The calibration curves of 26 pesticides were linear（correlatiom coefficient r0.99） within the range of 0.01 mg/L～0.5 mg/L.The recoveries ranged from 61%～95%,the relative standard deviations（RSD） of the method was 13% for each case,and the limit of determination（LOD） was 0.002 mg/kg～0.005 mg/kg.Conclusion： The method is suitable for determining organochlorine pesticide residues in animal food.

关 键 词：有机氯类农药 凝胶净化 气相色谱—质谱分析 选择离子监测方式 

分 类 号：O657.63[理学—分析化学]