引用本文:刘媛媛,张倩,梁涛,郑国砥,王凌青.加速溶剂萃取-在线净化-液相色谱串联质谱法检测污泥堆肥样品中三氯生和三氯卡班[J].环境监控与预警,2022,14(5):82-87
LIU Yuan-yuan, ZHANG Qian, LIANG Tao,ZHENG Guo-di, WANG Ling-qing.In cell Clean up Pressurized Liquid Extraction Liquid Chromatography Tandem Mass Spectrometry for the Analysis of TCS and TCC in Sewage Sludge[J].Environmental Monitoring and Forewarning,2022,14(5):82-87
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加速溶剂萃取-在线净化-液相色谱串联质谱法检测污泥堆肥样品中三氯生和三氯卡班
刘媛媛,张倩,梁涛,郑国砥,王凌青
中国科学院,地理科学与资源研究所,北京 100101
摘要:
污泥堆肥样品基质复杂,其中三氯生(TCS)和三氯卡班(TCC)的提取和净化过程操作烦琐、回收率低。通过对净化条件进行优化,建立了加速溶剂萃取-在线净化-液相色谱串联质谱法检测污泥堆肥样品中TCS和TCC的分析方法,并对上海某污水厂实际污泥堆肥样品中的TCS和TCC进行定量分析。结果表明,TCS和TCC的检出限分别为0.003和0.0002μg/g,加标回收率为90.3%~99.8%,相对标准偏差(RSD)为1.2%~8.5%(n=6)。该方法样品前处理时间短、回收率高、试剂使用量少,能够满足实际污泥堆肥样品中TCS和TCC的检测要求。
关键词:  污泥堆肥  加速溶剂萃取  在线净化  样品前处理  三氯生  三氯卡班
DOI:
分类号:X832
基金项目:国家自然科学基金—青年科学基金资助项目(42203011)
In cell Clean up Pressurized Liquid Extraction Liquid Chromatography Tandem Mass Spectrometry for the Analysis of TCS and TCC in Sewage Sludge
LIU Yuan-yuan, ZHANG Qian, LIANG Tao,ZHENG Guo-di, WANG Ling-qing
Institute of Geographic Sciences and Natural Resources Research, Chinese Academy of Sciences, Beijing 100101, China
Abstract:
The extraction and clean up of triclosan (TCS) and triclocarban (TCC) in sewage sludge is complicated and is of low recoveries. By optimizing the extraction conditions, an automated and sensitive method based on in cell clean up pressurized liquid extraction (PLE) coupled with liquid chromatography tandem mass spectrometry was developed for the determination of TCS and TCC in sewage sludge. The quantitative analysis on TCS and TCC in real sewage sludge samples from a sewage treatment plant in Shanghai was accomplished. The results showed that the limits of detection (LOD) were 0.003 and 0.000 2μg/g for TCS and TCC, respectively, and the recoveries were 90.3%~99.8% with relative standard deviations (RSD) ranged from 1.2% to 8.5% (n=6). The method is of less time consuming, higher recovery and less solvent usage. It meets the needs of determination of TCS and TCC in sewage sludge.
Key words:  Sewage sludge  Pressurized liquid extraction  In cell clean up  Pretreatment  TCC  TCS