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采用同位素稀释气相色谱-电子离子化串联质谱法分析水中的亚硝胺。

Analysis of N-nitrosamines in water by isotope dilution gas chromatography-electron ionisation tandem mass spectrometry.

机构信息

UNSW Water Research Centre, School of Civil and Environmental Engineering, University of New South Wales, NSW 2052, Australia.

出版信息

Talanta. 2012 Sep 15;99:146-54. doi: 10.1016/j.talanta.2012.05.032. Epub 2012 May 25.

Abstract

A method has been developed for the determination of eight N-nitrosamines in drinking water and treated municipal effluent. The method uses solid phase extraction (SPE), gas chromatography (GC) and analysis by tandem mass spectrometry (MS-MS) with electron ionization (EI). The target compounds are N-nitrosodimethylamine (NDMA), N-nitrosomethyethylamine (NMEA), N-nitrosodiethylamine NDEA), N-nitrosodipropylamine (NDPA), N-nitrosodi-n-butylamine (NDBuA), N-nitrosodiphenylamine (NDPhA), N-nitrosopyrrolidine (NPyr), N-nitrosopiperidine (NPip), N-nitrosomorpholine (NMorph). The use of direct isotope analogues for isotope dilution analysis of all analytes ensures accurate quantification, accounting for analytical variabilities that may occur during sample processing, extraction and instrumental analysis. Method detection levels (MDLs) were determined to describe analyte concentrations sufficient to provide a signal with 99% certainty of detection. The established MDLs for all analytes were 0.4-4 ng L(-1) in a variety of aqueous matrices. Sample matrices were observed to have only a minor impact on MDLs and the method validation confirmed satisfactory method stability over intra-day and inter-day analyses of tap water and tertiary treated effluent samples.

摘要

已开发出一种用于测定饮用水和处理后的城市污水中八种 N-亚硝胺的方法。该方法使用固相萃取 (SPE)、气相色谱 (GC) 和串联质谱 (MS-MS) 分析,并采用电子电离 (EI)。目标化合物为 N-亚硝基二甲胺 (NDMA)、N-亚硝基甲乙胺 (NMEA)、N-亚硝基二乙胺 (NDEA)、N-亚硝基二丙胺 (NDPA)、N-亚硝基二正丁胺 (NDBuA)、N-亚硝基二苯胺 (NDPhA)、N-亚硝基吡咯烷 (NPyr)、N-亚硝基哌啶 (NPip)、N-亚硝基吗啉 (NMorph)。使用直接同位素类似物进行所有分析物的同位素稀释分析可确保准确定量,可考虑到样品处理、提取和仪器分析过程中可能出现的分析变异性。方法检测限 (MDL) 用于描述足以提供 99%置信度检测信号的分析物浓度。在各种水基质中,所有分析物的建立 MDL 均为 0.4-4ng/L。观察到样品基质对 MDL 的影响较小,方法验证确认了该方法在自来水和三级处理后的污水样品的日内和日间分析中具有令人满意的稳定性。

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