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经 9-黄嘌呤衍生化后,用气相色谱-质谱法测定地表水中氨基甲酸酯类农药的痕量。

Trace level determinations of carbamate pesticides in surface water by gas chromatography-mass spectrometry after derivatization with 9-xanthydrol.

机构信息

Environmental Education Graduate School, Kongju National University, Kongju, 314-701, Republic of Korea.

出版信息

J Chromatogr A. 2013 Aug 30;1305:328-32. doi: 10.1016/j.chroma.2013.07.055. Epub 2013 Jul 19.

Abstract

A sensitive and selective gas chromatographic mass spectrometric method, based on derivatization with 9-xanthydrol, has been established for the simultaneous determination of five carbamate pesticides (carbaryl, carbofuran, metolcarb, isoprocarb and ethiofencarb) in surface water. 4-Bromo-3,5-dimethylphenyl-N-methylcarbamate was chosen as the internal standard for analyzing water samples. The derivatization of carbamates was performed directly in water and the reaction conditions (9-xanthydrol of 50.0mM, HCl concentration of 0.05M, reaction for 60min at 60°C) were established through the optimization of various parameters. Under the established conditions, the limits of quantification were in the range of 0.007-0.028μg/L, and the intra- and inter-day relative standard deviation were each less than 15% at concentrations of 0.1, 1.0 and 10μg/L. None of the carbamate pesticides were detected in any of the sixteen surface waters analyzed.

摘要

建立了一种基于 9-黄烷醇衍生化的灵敏、选择性气相色谱-质谱联用测定地表水中 5 种氨基甲酸酯农药(西维因、呋喃丹、涕灭威、异丙威和乙硫苯威)的方法。4-溴-3,5-二甲基苯基-N-甲基氨基甲酸酯被选为分析水样的内标。氨基甲酸酯的衍生化直接在水中进行,并通过优化各种参数确定了反应条件(50.0mM 9-黄烷醇、0.05M HCl 浓度、60°C 下反应 60min)。在建立的条件下,定量限在 0.007-0.028μg/L 范围内,在 0.1、1.0 和 10μg/L 浓度下,日内和日间相对标准偏差均小于 15%。在分析的 16 种地表水中均未检出任何氨基甲酸酯农药。

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