首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Determination of basic degradation products of chemical warfare agents in water using hollow fibre-protected liquid-phase microextraction with in-situ derivatisation followed by gas chromatography-mass spectrometry
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Determination of basic degradation products of chemical warfare agents in water using hollow fibre-protected liquid-phase microextraction with in-situ derivatisation followed by gas chromatography-mass spectrometry

机译:中空纤维保护液相微萃取-原位衍生化-气相色谱-质谱法测定水中化学战剂的基本降解产物

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摘要

Hollow fibre-protected liquid-phase microextraction (HF-LPME) together with gas chromatography-mass spectrometry was, for the first time, investigated for the in-situ derivatisation and analysis of basic degradation products of chemical warfare agents in water samples. The degradation products studied were those of nerve and blister agents, and a psychotomimetic agent. Extractions with in-situ derivatisation were successfully performed using a mixture of solvent and derivatising agent. The protection of the moisture-sensitive derivatising agent was afforded by the hydrophobic hollow fibre. Parameters such as type of derivatising agent, extraction solvent, pH, salt concentration, stirring speed and extraction time were optimised using spiked deionised water samples. The linear range established was between 0.05 and 25 mu g ml(-1) depending on analyte, with squared regression coefficients ranging from 0.9959 to 0.9996. Relative standard deviations (RSDs) ranged from 6% to 10%. As comparison, solid-phase microextraction (SPME) was also evaluated and extraction conditions such as pH, salt concentration, stirring speed and extraction time were optimised. This work also represented the first report of such an in-situ derivatisation approach for SPME of basic analytes. The linear range established was between 0.5 and 25 mu g ml(-1) depending on analyte, with squared regression coefficients ranging from 0.9946 to 0.9998. RSDs ranged from 5% to 22%. The limits of detection of HF-LPME (0.04-0.36 mu g l(-1)) showed improvement over those of SPME (0.06-0.77 mu g l(-1)). (C) 2008 Elsevier B.V. All rights reserved.
机译:空心纤维保护液相微萃取(HF-LPME)与气相色谱-质谱联用,是首次用于原位衍生化和分析水样品中化学战剂的基本降解产物。研究的降解产物是神经和起泡剂以及拟精神药的降解产物。使用溶剂和衍生剂的混合物成功进行了原位衍生化萃取。疏水性中空纤维提供了对湿敏性衍生剂的保护。使用加标的去离子水样品优化了诸如衍生剂类型,萃取溶剂,pH,盐浓度,搅拌速度和萃取时间等参数。根据分析物的不同,建立的线性范围为0.05至25μg ml(-1),回归系数的平方范围为0.9959至0.9996。相对标准偏差(RSD)为6%至10%。作为比较,还对固相微萃取(SPME)进行了评估,并优化了萃取条件,例如pH,盐浓度,搅拌速度和萃取时间。这项工作也代表了这种针对碱性分析物SPME的原位衍生化方法的首次报道。建立的线性范围介于0.5到25μg ml(-1)之间,具体取决于分析物,回归系数的平方范围为0.9946至0.9998。 RSD范围从5%到22%。 HF-LPME(0.04-0.36μg l(-1))的检出限显示出比SPME(0.06-0.77μg l(-1))的检出限有所改善。 (C)2008 Elsevier B.V.保留所有权利。

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