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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
In-cell Clean-up-Pressurized Liquid Extraction-Liquid Chromatography-Tandem Mass Spectrometry for the Analysis of TCS and TCC in Sewage Sludge
【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0.000 2μg/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。
【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 2 μg/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;
- 【文献出处】 环境监控与预警 ,Environmental Monitoring and Forewarning , 编辑部邮箱 ,2022年05期
- 【分类号】O657.63;X830.2
- 【下载频次】69