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索氏提取固体环境样品过程中产生的丙酮 - 己烷假象分析

Analysis of acetone-hexane artifacts produced in the Soxhlet extraction of solid environmental samples.

作者信息

Hunchak K, Suffet I H

出版信息

J Chromatogr. 1987 Apr 17;392:185-98. doi: 10.1016/s0021-9673(01)94265-7.

Abstract

A study was performed to examine the artifact formation during the acetone-hexane Soxhlet extraction of suspended materials collected on glass fiber filters. Capillary gas chromatographic analysis showed a great number of artifacts of significant concentration in the Soxhlet extractions of the filters after cleaning, the acetone solvent blank and the acetone-hexane Soxhlet blank. Gas chromatographic-mass spectrometric analysis indicated that the compounds are primarily condensation products of acetone produced during the Soxhlet extraction process and solvent impurities. Acetone and hexane washes of the glass fiber filters showed a large variety of compounds to be present on the filters as received from the manufacturer. A reaction scheme is proposed to explain the formation of some of the acetone condensation products identified in this study. A comparison study using methylene chloride to clean and extract the filters showed considerably less artifact formation and solvent impurities. The development of an appropriate quality assured extraction method, which minimizes artifact formation, is needed for the broad spectrum analysis of non-polar trace organics associated with suspended materials in aquatic samples.

摘要

开展了一项研究,以检测在对玻璃纤维滤膜上收集的悬浮物质进行丙酮 - 己烷索氏提取过程中伪像的形成情况。毛细管气相色谱分析表明,在清洗后的滤膜、丙酮溶剂空白样以及丙酮 - 己烷索氏提取空白样的索氏提取物中存在大量具有显著浓度的伪像。气相色谱 - 质谱分析表明,这些化合物主要是索氏提取过程中产生的丙酮缩合产物以及溶剂杂质。对玻璃纤维滤膜进行丙酮和己烷冲洗后发现,从制造商处收到的滤膜上存在大量不同的化合物。提出了一个反应方案来解释本研究中鉴定出的一些丙酮缩合产物的形成过程。一项使用二氯甲烷清洗和提取滤膜的对比研究表明,伪像形成和溶剂杂质明显更少。对于水生样品中与悬浮物质相关的非极性痕量有机物进行广谱分析,需要开发一种适当的质量保证提取方法,以尽量减少伪像的形成。

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