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使用气相色谱-离子阱质谱法对污水污泥中多环芳烃进行定量分析的各种萃取技术的验证

Validation of various extraction techniques for the quantitative analysis of polycyclic aromatic hydrocarbons in sewage sludges using gas chromatography-ion trap mass spectrometry.

作者信息

Helaleh Murad I H, Al-Omair Ali, Nisar A, Gevao B

机构信息

Kuwait Institute for Scientific Research (KISR), Central Analytical Laboratory (CAL), P.O. Box, Safat, Kuwait.

出版信息

J Chromatogr A. 2005 Aug 12;1083(1-2):153-60. doi: 10.1016/j.chroma.2005.05.085.

Abstract

A new GC-ion trap MS method has been developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge samples. The sludge samples were extracted with Soxhlet, Soxtec, and pressurized liquid extraction (PLE) using 1:1 (v/v) dichloromethane (DCM):n-hexane solvent mixture. A multi-layer clean-up (silica/Al2O3) column were used, followed by gel permeation chromatography (GPC) to eliminate the interfering organic compound as well as the lipids. The extracts were quantified with GC-EI-SIS and GC-EI-MS-MS. The method was successfully applied to determine the concentration of PAHs present in sewage sludge samples collected from four waste water treatment plants (WWTPs). The method recovery values varied from 61.5 to 90.5%, 65.0 to 91.8% and 60.0 to 93.4% for Soxtec extraction, Soxhlet extraction and PLE extraction, respectively. The total concentrations of the 16 PAHs in the sewage sludge samples were found to vary from 1.56 to 6.18 mg/kg. The concentration of PAHs in WWTPs did not significantly vary.

摘要

已开发出一种新的气相色谱-离子阱质谱法,用于测定污水污泥样品中的多环芳烃(PAHs)。污泥样品采用索氏提取法、索格利特提取法和加压液体萃取法(PLE),以1:1(v/v)二氯甲烷(DCM):正己烷溶剂混合物进行提取。使用多层净化(硅胶/Al2O3)柱,随后进行凝胶渗透色谱法(GPC)以去除干扰性有机化合物和脂质。提取物通过气相色谱-电子轰击-选择离子监测(GC-EI-SIS)和气相色谱-电子轰击-串联质谱(GC-EI-MS-MS)进行定量。该方法成功应用于测定从四个污水处理厂(WWTPs)采集的污水污泥样品中PAHs的浓度。索格利特提取法、索氏提取法和PLE提取法的方法回收率分别为61.5%至90.5%、65.0%至91.8%和60.0%至93.4%。污水污泥样品中16种PAHs的总浓度在1.56至6.18 mg/kg之间。污水处理厂中PAHs的浓度没有显著差异。

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