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采用固相萃取和带化学电离串联质谱的气相色谱法分析纳克/升低浓度饮用水中N-亚硝基二甲胺及其他N-亚硝胺的方法开发

Method development for the analysis of N-nitrosodimethylamine and other N-nitrosamines in drinking water at low nanogram/liter concentrations using solid-phase extraction and gas chromatography with chemical ionization tandem mass spectrometry.

作者信息

Munch Jean W, Bassett Margarita V

机构信息

U.S. Environmental Protection Agency, Office of Research and Development, National Exposure Research Laboratory, MS-564, 26 W. Martin Luther King Dr, Cincinnati, OH 45268, USA.

出版信息

J AOAC Int. 2006 Mar-Apr;89(2):486-97.

Abstract

N-nitrosodimethylamine (NDMA) is a probable human carcinogen of concern that has been identified as a drinking water contaminant. U.S. Environmental Protection Agency Method 521 has been developed for the analysis of NDMA and 6 additional N-nitrosamines in drinking water at low ng/L concentrations. The method uses solid-phase extraction with coconut charcoal as the sorbent and dichloromethane as the eluent to concentrate 0.50 L water samples to 1 mL. The extracts are analyzed by gas chromatography-chemical ionization tandem mass spectrometry using large-volume injection. Method performance was evaluated in 2 laboratories. Typical analyte recoveries of 87-104% were demonstrated for fortified reagent water samples, and recoveries of 77-106% were demonstrated for fortified drinking water samples. All relative standard deviations on replicate analyses were < 11%.

摘要

N-亚硝基二甲胺(NDMA)是一种备受关注的可能的人类致癌物,已被确定为饮用水污染物。美国环境保护局已制定了方法521,用于分析饮用水中低纳克/升浓度的NDMA和另外6种N-亚硝基胺。该方法采用以椰壳炭为吸附剂、二氯甲烷为洗脱剂的固相萃取法,将0.50升水样浓缩至1毫升。提取物通过气相色谱-化学电离串联质谱法采用大体积进样进行分析。在2个实验室对方法性能进行了评估。对于加标试剂水样,典型分析物回收率为87%-104%,对于加标饮用水样,回收率为77%-106%。重复分析的所有相对标准偏差均<11%。

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