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柱前用苯甲酰氯衍生化后,采用反相液相色谱法测定水中主要酚类化合物。

Determination of major phenolic compounds in water by reversed-phase liquid chromatography after pre-column derivatization with benzoyl chloride.

作者信息

Asan Adem, Isildak Ibrahim

机构信息

Department of Chemistry. Faculty of Science, Ondokuzmayis University, 55139 Kurupelit-Samsun, Turkey.

出版信息

J Chromatogr A. 2003 Feb 21;988(1):145-9. doi: 10.1016/s0021-9673(02)02056-3.

Abstract

A simple reversed-phase LC method capable of detecting ng/ml quantities of phenolic compounds in water is described. Pre-column derivatization with benzoyl chloride is used for the separation and determination o-cresol, m-cresol, p-cresol, phenol, resorcinol, catechol and hydroquinone in water. The benzoyl derivatives formed within in 15 min, were extracted with dietyl ether, and then analyzed by liquid chromatography with UV detection at 232 nm. With a mobile phase of acetonitrile-tetrahydrofuran-water (54:6:40, v/v) the seven derivatives were eluted in 15 min. The detection limits were between 0.05 and 0.50 ng/ml for 50 ml of a standard water sample. The method was applied to the analysis of phenols in wine and river water. The recovery of the derivatives from pure water was 81-94% with relative standard deviations of 2.5-5.0%.

摘要

本文描述了一种简单的反相液相色谱法,该方法能够检测水中纳克/毫升级别的酚类化合物。采用苯甲酰氯进行柱前衍生化,用于分离和测定水中的邻甲酚、间甲酚、对甲酚、苯酚、间苯二酚、儿茶酚和对苯二酚。15分钟内形成的苯甲酰衍生物用二乙醚萃取,然后通过液相色谱在232nm处进行紫外检测分析。以乙腈 - 四氢呋喃 - 水(54:6:40,v/v)为流动相,七种衍生物在15分钟内洗脱。对于50毫升标准水样,检测限在0.05至0.50纳克/毫升之间。该方法应用于葡萄酒和河水中酚类的分析。衍生物从纯水中的回收率为81 - 94%,相对标准偏差为2.5 - 5.0%。

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