污水处理系统中三氯生固相萃取(SPE气)-相色谱(GC)-电子俘获检测器(ECD)测定方法的建立和优化  

ESTABLISHMENT AND OPTIMIZATION OF DETERMINATION METHOD FOR TRICLOSAN WITH SPE-GC-ECD IN THE WASTEWATER TREATMENT SYSTEM

作　　者：周雪飞[1] 陈家斌[1] 周世兵[2] 张亚雷[2] 石璐[2] 

机构地区：[1]同济大学环境学院长江水环境教育部重点实验室,上海200092 [2]同济大学污染控制与资源化国家重点实验室,上海200092

出　　处：《环境化学》2011年第2期506-510,共5页Environmental Chemistry

基　　金：教育部新世纪优秀人才支持计划(NCET-07-0627);国家科技支撑计划(2006BAJ08B00);上海市国际科技合作基金(072307007)资助

摘　　要：建立了污水处理系统中三氯生的固相萃取(SPE)-气相色谱分离(GC)-ECD检测器检测的分析方法.采集和处理水样和泥样后,优化了三氯生衍生化条件,即衍生化试剂量为150μL,反应温度为70℃,反应时间为120 min;GC-ECD对三氯生的方法检出限可达0.56μg.L-1(S/N=3),定量检出限为1.22μg.L-1(S/N=10),回收率在90%左右,相对标准偏差(RSD)在1.5%—3.9%之间(n=6),能够满足痕量物质三氯生的检测需要.该方法应用到测定上海市两座污水处理厂水样和泥样中三氯生含量,进水中三氯生浓度分别为1287ng.L-1和2086 ng.L-1,污泥中三氯生含量为1530μg.kg-1和2563μg.kg-1.A analytical method was developed for the determination of triclosan with solid-phase extraction（SPE） followed by gas chromatography（GC）-electron capture detector（ECD）.After collection and enrichment of sewage and sludge sample,the optimization of derivatization condition and determination of triclosan was performed.The optimal derivatization was 150μL derivatization reagent,120min reaction at 70℃.The method detection limit and quantitative detection limit were 0.56 μg·L^-1（S/N=3） and 1.22 μg·L^-1（S/N=10）,respectively.The average recovery was about 90%,and the relative standard deviation（RSD） ranged between 1.5% and 3.9%.The optimized method was applied to investigate the occurrence of triclosan in two wastewater treatment plants in Shanghai.The concentration of triclosan in the influent was 1287 and 2086 ng·L^-1,respectively,and the triclosan content in the excess sludge was 1530 and 2563 μg·kg^-1.

关 键 词：药物和个人护理品 三氯生 衍生化 气相色谱法 

分 类 号：X832[环境科学与工程—环境工程]