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通过循环蒸汽蒸馏萃取后,采用气相色谱/质谱法测定环境样品中的半挥发性有机化合物。

Determination of semivolatile organic compounds in environmental samples by gas chromatography/mass spectrometry after extraction by cyclic steam distillation.

作者信息

Kawata Kuniaki, Tanabe Akiko, Yagoh Hiroaki, Ibaraki Tsuyoshi, Yasuhara Akio, Shibamoto Takayuki

机构信息

Niigata Prefectural Institute of Public Health and Environmental Sciences, 314-1 Sowa, Niigata 950-2144, Japan.

出版信息

J AOAC Int. 2003 Mar-Apr;86(2):246-56.

PMID:12723913
Abstract

A method was developed for the multiple determination of semivolatile organic compounds found in groundwater, river water, seawater, sediment, and soil. Forty standard compounds were determined: n-alkenes, cycloalkanes, aromatic hydrocarbons, and polycyclic aromatic hydrocarbons. The compounds were isolated from water and soil samples by using an essential oil distillator (cyclic steam distillator) with hexane as a solvent. The extract was cleaned by using a silica gel cartridge with an acetone-hexane solution. The compounds were determined by using a gas chromatograph/mass spectrometer with 12 stable isotope-labeled compounds (surrogate compounds). The efficiencies of recoveries from water samples were 80.0-106% for groundwater, 80.1-106% for river water, and 81.2-103% for seawater. The relative standard deviation (RSD) values were 2.05-16.0% for groundwater, 3.22-16.6% for river water, and 4.45-16.0% for seawater. The efficiencies of recoveries from sediment and soil were 71.5-96.4% and 70.1-99.8%, respectively. RSD values ranged from 2.27 to 16.0% for sediment and from 2.12 to 15.1% for soil. Adjustment of recovery efficiencies of standard compounds by using surrogate compounds gave more accurate values. The present study proved that an essential oil distillator provides satisfactory results for multiple determinations of the semivolatile compounds in environmental waters, sediment, and soil.

摘要

开发了一种用于多重测定地下水、河水、海水、沉积物和土壤中半挥发性有机化合物的方法。测定了40种标准化合物:正构烯烃、环烷烃、芳烃和多环芳烃。通过使用精油蒸馏器(循环蒸汽蒸馏器),以己烷为溶剂,从水和土壤样品中分离出这些化合物。提取物用装有丙酮 - 己烷溶液的硅胶柱进行净化。使用配备12种稳定同位素标记化合物(替代化合物)的气相色谱/质谱仪测定这些化合物。水样的回收率效率为:地下水80.0 - 106%,河水80.1 - 106%,海水81.2 - 103%。相对标准偏差(RSD)值为:地下水2.05 - 16.0%,河水3.22 - 16.6%,海水4.45 - 16.0%。沉积物和土壤的回收率效率分别为71.5 - 96.4%和70.1 - 99.8%。沉积物的RSD值范围为2.27至16.0%,土壤的RSD值范围为2.12至15.1%。使用替代化合物调整标准化合物的回收率可得到更准确的值。本研究证明,精油蒸馏器对于环境水、沉积物和土壤中半挥发性化合物的多重测定提供了令人满意的结果。

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