加速溶剂萃取-气相色谱/质谱法测定土壤中多氯代烃和有机磷阻燃剂  

Determination of polychlorinated hydrocarbons and organophosphorus flame retardants in soil by accelerated solvent extraction combined with gas chromatography-tandem mass spectrometry

作　　者：许颖藻 陈智锋 祁增华 蔡宗苇[1,2] XU Yingzao;CHEN Zhifeng;QI Zenghua;CAI Zongwei(Guangdong-Hong Kong-Macao Joint Laboratory for Contaminants Exposure and Health,School of Environmental Science and Engineering,Guangdong University of Technology,Guangzhou 510006,China;State Key Laboratory of Environmental and Biological Analysis,Department of Chemistry,Hong Kong Baptist University,Hong Kong 999077,China)

机构地区：[1]广东工业大学环境科学与工程学院,粤港澳污染物暴露与健康联合实验室,广州510006 [2]香港浸会大学化学系,环境与生物分析国家重点实验室,中国香港999077

出　　处：《分析试验室》2022年第6期628-634,共7页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划项目(2019YFC1804604);广东省自然科学基金(2021A1515010018);广东省科技计划项目(2020B1212030008)资助。

摘　　要：建立了加速溶剂萃取-气相色谱/质谱(ASE-GC-MS/MS)测定土壤中6种多氯代烃(PCHs)和12种有机磷阻燃剂(OPFRs)的方法,对加标制样、净化和仪器分析条件进行了优化。在土样与硅藻土混合物中加入回收内标混合液后,用加速溶剂萃取同时提取6种PCHs和12种OPFRs,固相萃取分步净化,气相色谱联用质谱仪测定。结果表明,目标分析物质量分数在0.05~500 ng/g范围内,相关系数(r^(2))>0.995,PCHs和OPFRs的方法检出限分别为0.16~2.31 pg/g和4.25~21.5 pg/g,方法定量限分别为0.533~7.71 pg/g和14.2~71.6 pg/g。PCHs和OPFRs的平均回收率分别为62.6%~111.0%和65.9%~119.2%。该方法适用于土壤中6种PCHs和12种OPFRs的检测。A method was established for the determination of 6 polychlorinated hydrocarbons(PCHs)and 12 organophosphorus flame retardants(OPFRs)in soils by accelerated solvent extraction combined with gas chromatography-tandem mass spectrometry(ASE-GC-MS/MS).In this paper,the sample preparation,purification procedure and instrumental parameter were optimized.The mixture samples of soil and diatomite were spiked with mixed internal standard solution.Thereafter,6 PCHs and 12 OPFRs were extracted simultaneously by accelerated solvent extraction,purified by solid-phase extraction and determined by gas chromatography-tandem mass spectrometry.The results showed that the calibration curves of all target compounds with good correlation coefficients(r~2>0.995)were mostly obtained in the range of 0.05-500 ng/g.The method detection limits(MDL)of PCHs and OPFRs were in the ranges of 0.16-2.31 pg/g and 4.25-21.5 pg/g,as well as the method quantification limits(MQL) were 0.533-7.71 pg/g and 14.2-71.6 pg/g for PCHs and OPFRs,respectively.The average recoveries of PCHs and OPFRs were 62.6%-111.0% and 65.9%-119.2%,respectively.This developed method is suitable for the detection of 6 PCHs and 12 OPFRs in soil samples.

关 键 词：土壤 多氯代烃 有机磷阻燃剂 加速溶剂萃取 气相色谱联用质谱 

分 类 号：O657.63[理学—分析化学]