加速溶剂提取/GC-MS同时测定动物组织中有机氯农药和多氯联苯  

Simultaneous Analysis of Organochlorinated Pesticides and Polychlorinated Biphenyls from Animal Tissue using Gas Chromatography-Mass Spectrometry Combined with Accelerated Solvent Extraction

作　　者：佟玲[1] 杨佳佳[1] 阎妮[2] 吴淑琪[1] 

机构地区：[1]国家地质实验测试中心,北京100037 [2]中国地质大学(北京)水资源与环境学院,北京100083

出　　处：《岩矿测试》2014年第2期262-269,共8页Rock and Mineral Analysis

基　　金：中国地质调查局地质调查工作项目(1212010816028);国土资源公益性行业科研专项(200911044-02-2)

摘　　要：动物组织样品油脂含量大、干扰杂质多,对其中低含量有机氯农药及多氯联苯的分析会造成较大程度的影响.针对动物组织样品基质复杂的特点,本文以二氯甲烷-丙酮（体积比为1∶1）的溶剂体系,采用加速溶剂萃取技术对样品进行提取,在提取过程中尽量减少脂肪的共提出,然后采用凝胶渗透色谱技术去除样品中的大部分油脂,再结合弗罗里硅土为填料的固相萃取方法对样品进一步净化,能够达到充分去除油脂和小分子杂质的目的.采用气相色谱-质谱分析17种有机氯农药及7种指示性多氯联苯,各化合物的回收率在81.6％～113.4％之间,检出限在1.02～3.59 ng/g之间,技术指标优于部分国家标准.本方法改进了动物样品的净化效果,建立了凝胶渗透色谱结合固相萃取技术的净化方法,达到了样品快速自动提取、溶剂用量少、基质净化彻底的目的,降低了方法检出限,能够满足快速、准确检测动物组织中低含量持久性有机污染物的要求.The majority of fat and impurities in animal tissues influence the analysis result for low concentration organic compounds.To overcome this issue,the animal sample was extracted by accelerated solvent extraction （ASE） with methylene chloride/acetone （Ⅴ ∶ Ⅴ =1 ∶ 1）,which reduced the co-extraction lipids during the extraction process.Gel Permeation Chromatography （GPC） combined with solid phase extraction （SPE） was applied to remove lipids from the sample solution.The GPC can remove most of the macromolecular lipids in samples,and the SPE with florisil can sufficiently reduce fat and small molecule impurity.The accuracy and sensitivity of the method can be improved by this pretreatment process.The compounds,including 17 organochlorinated pesticides and 7 indicator polychlorinated biphenyls in animal tissue,can be simultaneously analysed by Gas Chromatography Mass Spectrometry.The recoveries of 25 of the target compounds were in the range of 81.6%-113.4% and the method detection limits for dry samples were 1.02-3.59 ng/g.These results were superior to those of the national standard.This method improved the purification effect of animal samples,reduced the method detection limit,and enhanced the accuracy.It can be used to quickly and accurately determine the low content of persistent organic pollutants in animals.

关 键 词：动物组织 有机氯农药 多氯联苯 加速溶剂萃取 凝胶渗透色谱 固相萃取 气相色谱-质谱法 

分 类 号：S482.32[农业科学—农药学] O625.21[农业科学—植物保护]