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采用微固相萃取结合液相色谱-质谱检测法测定处理水中低分子量取代苯甲醛。

Trace determination of low-molecular-mass substituted benzaldehydes in treated water using micro solid-phase extraction followed by liquid chromatography-mass spectrometric detection.

机构信息

Department of Analytical Chemistry, Marie-Curie Building (Annex), Rabanales Campus, University of Cordoba, E-14071 Cordoba, Spain.

出版信息

J Chromatogr A. 2013 Jul 26;1300:180-6. doi: 10.1016/j.chroma.2013.05.048. Epub 2013 May 28.

Abstract

Aldehydes are a class of water disinfection by-products (DBPs) that are an object of special attention due to their high toxicity and carcinogenic effect. While aliphatic low-molecular-mass aldehydes (LMMAs) are often measured in waters, there is little information on the occurrence of aromatic LMMAs. This paper reports the development of a simple, rapid and sensitive method for the quantitative determination of six LMM substituted benzaldehydes (BAs) as DBPs in treated water. The method is based on the continuous in situ derivatisation/extraction of aldehydes on a Telos™ ENV μ-solid-phase extraction (μ-SPE) column impregnated with 2,4-dinitrophenylhydrazine (DNPH). After elution of the hydrazones with acetonitrile (ACN), the derivatives are analysed using liquid chromatography-mass spectrometry (LC-MS). Under optimum conditions, limits of detection (LODs) were obtained between 15 and 25ng/L and the inter-day precision expressed as the relative standard deviation (RSD) ranged from 6.1% to 7.7%. Matrix effects were shown to be negligible by comparing the response factors (RFs) obtained in ultra-pure and treated waters. The proposed method is the first contribution developed for the analysis of LMM substituted BAs as DBPs in waters by LC-MS. Some of the aromatic LMMAs identified had not previously been reported for swimming pool water.

摘要

醛类是一类水消毒副产物(DBPs),由于其高毒性和致癌作用,受到特别关注。虽然脂肪族低分子量醛(LMMAs)通常在水中进行测量,但关于芳香族 LMMAs 的发生情况知之甚少。本文报道了一种简单、快速和灵敏的方法,用于定量测定作为处理水中 DBPs 的六种 LMM 取代苯甲醛(BAs)。该方法基于 Telos™ENV μ-固相萃取(μ-SPE)柱上的原位衍生/萃取醛,该柱中浸渍有 2,4-二硝基苯肼(DNPH)。用乙腈(ACN)洗脱腙后,用液相色谱-质谱法(LC-MS)分析衍生物。在最佳条件下,检测限(LODs)在 15 到 25ng/L 之间,日内精密度表示为相对标准偏差(RSD)在 6.1%到 7.7%之间。通过比较超纯水和处理水中获得的响应因子(RFs),表明基质效应可以忽略不计。该方法是第一个通过 LC-MS 分析水中 LMM 取代 BAs 作为 DBPs 的方法。一些鉴定出的芳香族 LMMAs 以前没有报道过用于游泳池水。

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