微波辅助萃取法提取滇池沉积物中的多氯联苯  

MICROWAVE-ASSISTED EXTRACTION OF PCBS IN SEDIMENT FROM DIANCHI LAKE

作　　者：万幸[1] 王彬[1] 赵世民[1,2] 胡平[2] 李发荣[2] 潘学军[1] 

机构地区：[1]昆明理工大学环境科学与工程学院,昆明650093 [2]昆明市环境监测中心,昆明650093

出　　处：《环境化学》2011年第10期1781-1787,共7页Environmental Chemistry

基　　金：国家自然科学基金(20767002);云南省自然科学基金(2007B035M);环境化学与生态毒理学国家重点实验室开放基金(KF2008-09号)资助

摘　　要：研究运用微波辅助萃取-固相萃取-气相色谱/质谱检测滇池沉积物中6种指示性多氯联苯(PCB28、PCB52、PCB101、PCB138、PCB153和PCB180).重点优化了微波辅助萃取技术,在萃取温度为100℃和萃取时间为30 min(升温和恒温各15 min)条件下,以30 mL正己烷∶二氯甲烷(1∶1,V∶V)的混合溶液为萃取溶剂,萃取5 g加标沉积物样品.本方法对PCB28、PCB52、PCB101和PCB138、PCB153、PCB180的线性范围分别为1—3000 pg.g(d.w.)-1和5—3000 pg.g(d.w.)-1,相关系数R2>0.98,检出限和定量限分别为41.7—62.3pg.g(d.w.)-1、139.0—207.7 pg.g(d.w.)-1.浓度水平为20 ng·g(d.w.)-1的滇池沉积物样品平均加标回收率在75.1%—93.9%之间,相对标准偏差为3.9%—12.8%(n=3).运用该方法对滇池环境样品进行了测定,结果表明滇池表层沉积物已受到多氯联苯的污染.A method for simultaneous determination of six indicative polychlorinated biphenyls（PCB28,PCB52,PCB101,PCB138,PCB153 and PCB180） in sediments of Dianchi Lake by microwave-assisted extraction（MAE）,solid phase extraction（SPE） and gas chromatography-mass spectrometry（GC-MS） detection was developed.Based on systematic optimization of MAE conditions,the most efficient extraction was achieved at 100 ℃ for 30 min（heating for 15 min and then holding for 15 min）,using 30 mL of hexane∶DCM（1∶1,V∶V） as the solvent for 5 g sediment sample.Under the optimal conditions,linear range was 1—3000 pg·g（dry weight）-1 for PCB28,PCB52 and PCB101,while 5—3000 pg·g（dry weight）-1 for PCB138,PCB153 and PCB180.The correlation coefficient（R2） was above 0.98 for all the analytes,with the limit of detection（LOD） and the limit of quantification（LOQ） of 41.7—62.3 pg·g（dry weight）-1 and 139.0—207.7 pg·g（dry weight）-1,respectively.The proposed method was further verified by performing spiking experiments in sediment samples at 20 ng·g（dry weight）-1,with the overall recoveries ranging from 75.1% to 93.9% and relative standard deviations（RSD）（n=3） of 3.9%—12.8% for the entire procedure.The proposed method was applied to the determination of PCBs in surface sediment samples from Dianchi Lake,showing that the sediment had been contaminated by PCBs.

关 键 词：多氯联苯 沉积物 微波辅助萃取 

分 类 号：X524[环境科学与工程—环境工程] X13