气相色谱-质谱法同时测定河流沉积物中多环芳烃和有机氯农药  

Simultaneous Determination of Polycyclic Aromatic Hydrocarbons and Organochlorine Pesticides in River Sediments by Gas Chromatography-Mass Spectrometry

作　　者：汪瑾彦[1] 汤桦[2] 陈大舟[2] 吴雪[2] 冯洁[1] 吴学丽[3] 李蕾[1] 

机构地区：[1]北京化工大学理学院,北京100029 [2]中国计量科学研究院化学计量与分析科学研究所,北京100013 [3]国家地质实验测试中心,中国地质科学院生态地球化学重点开放实验室,北京100037

出　　处：《岩矿测试》2010年第3期225-230,共6页Rock and Mineral Analysis

基　　金：科技部科技基础性工作专项资助(21-08-4GZ-5);科技部国际合作项目资助(2006DFA21280);国家自然科学基金项目资助(40773010)

摘　　要：建立了用加速溶剂萃取,气相色谱-质谱法同时测定河流沉积物中16种多环芳烃和19种有机氯农药的分析方法,优化了萃取溶剂、萃取温度和时间、凝胶渗透色谱收集时间、固相萃取洗脱溶剂和洗脱体积等条件。16种多环芳烃的方法检出限在0.15~0.59 ng/g,加标回收率为82%~102%,相对标准偏差（RSD,n=5）为1.1%~4.5%。19种有机氯农药的方法检出限在0.14~2.23 ng/g,加标回收率为71%~108%,相对标准偏差（RSD,n=5）为1.0%~4.5%。实际样品的测定结果表明,该方法分离效果较好,能够满足沉积物样品中多环芳烃和有机氯农药的分析要求。A method for simultaneous determination of 16 polycyclic aromatic hydrocarbons（PAHs） and 19 organochlorine pesticides（OCPs） in river sediments by gas chromatography-mass spectrometry with accelerated solvent extraction（ASE） was established.The parameters of ASE,such as type of extraction solvent,extraction temperature and time,the collection time for gel permeation chromatograph,as well as the selection of elution agents and elution parameters in solid phase extraction（SPE） were optimized.The detection limits for 16 PAHs ranged from 0.15 to 0.59 ng/g（dry weight）,and the recoveries for spiked samples were between 82% and 102% with precision of 1.1%～4.5% RSD（n=5）.The detection limits for 19 OCPs ranged from 0.14～2.23 ng/g（dry weight）,and the recoveries for spiked samples were between 71% and 108% with precision of 1.0%～4.5% RSD（n=5）.The method has been applied to the determination of 16 PAHs and 19 OCPs in sediment samples with satisfactory results.

关 键 词：加速溶剂萃取 气相色谱-质谱法 沉积物 多环芳烃 有机氯农药 

分 类 号：O652.62[理学—分析化学] O657.63[理学—化学]