固相萃取-气相色谱法测定海水中狄氏剂和多氯联苯  

Determination of Dieldrin and Polychlorinated Biphenyls in Seawater by Solid Phase Extraction and Capillary Gas Chromatography

作　　者：刘静[1] 王丽[2] 曾兴宇[1] 张艳萍[1] 王旭亮[1] 

机构地区：[1]国家海洋局天津海水淡化与综合利用研究所,天津300192 [2]天津市第一轻工业学校,天津300130

出　　处：《岩矿测试》2014年第2期282-286,共5页Rock and Mineral Analysis

基　　金：海洋公益性行业科研专项经费项目(201305039);中央级公益性科研院所基本科研业务费专项资金项目(K-JBYWF-2012-G11)

摘　　要：狄氏剂与多氯联苯均是海洋环境中毒性大、难降解的有机污染物,建立海水中狄氏剂与多氯联苯快速、灵敏、准确的检测方法,具有重要意义.本文采用聚苯乙烯/二乙烯基苯（Cleanert PS）固相萃取柱对海水样品中的狄氏剂与7种多氯联苯进行分离富集,建立了气相色谱-电子捕获检测器（GC-μECD）的分析方法.实验了萃取流速、洗脱液、水样盐度与pH等实验条件对萃取效率的影响,确定样品以5.0 mL/min的流速经Cleanert PS固相萃取柱富集,真空抽干后用5.0 mL丙酮洗脱,挥干洗脱液,用1.0 mL正己烷定容,在选定的色谱条件下进行分析.方法精密度（RSD）为0.9％～4.4％,加标回收率为82.1％～123.9％.狄氏剂的检出限为0.0088 μg/L,7种多氯联苯的检出限为0.0012～0.0067 μg/L.该方法适合于海水中痕量狄氏剂与多氯联苯的快速分析,具有一定的实用价值.Dieldrin and polychlorinated biphenyls （PCBs） are toxic,organic pollutants that break down extremely slowly in the marine environment.Therefore,it is of valuable significance to establish a rapid,sensitive and accurate detection method for dieldrin and PCBs in seawater.A method has been developed for determining dieldrin and seven PCBs in seawater by Cleanert PS solid-phase extraction and capillary Gas Chromatography with an Electron Capture Detector （GC-μECD）.Determination parameters,such as extracting flow rate,eluent,seawater salinity and pH and their effects for extraction efficiency are discussed.By the new method,dieldrin and seven PCBs were extracted from seawater under a flow rate of 5.0 mL/min,eluted by 5.0 mL acetone.The eluate was evaporated,and the solvent was set to 1.0 mL with hexane.The target compounds were determined by GC-μECD.The average recoveries of the method ranged from 82.1% to 123.9%,and has a better precision with relative standard deviation （RSD） of 0.9%-4.4%.The detection limit of dieldrin was 0.0088 μg/L.Meanwhile,the detection limits of 7 kinds of PCBs range from were 0.0012 to 0.0067 μg/L.The established method was qualified for rapid determination of dieldrin and PCBs in seawater samples with a good practical value.

关 键 词：海水 狄氏剂 多氯联苯 固相萃取 气相色谱法 

分 类 号：P641[天文地球—地质矿产勘探] O625.21[天文地球—地质学]