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采用中空纤维保护的液相微萃取结合气相色谱-质谱联用技术测定水和泥浆样品中的痕量化学战剂。

Determination of trace level chemical warfare agents in water and slurry samples using hollow fibre-protected liquid-phase microextraction followed by gas chromatography-mass spectrometry.

作者信息

Lee Hoi Sim Nancy, Basheer Chanbasha, Lee Hain Kee

机构信息

DSO National Laboratories, Singapore.

出版信息

J Chromatogr A. 2006 Aug 18;1124(1-2):91-6. doi: 10.1016/j.chroma.2006.05.030.

Abstract

A simple and solvent-minimised sample preparation technique based on hollow fibre-protected liquid-phase microextraction was investigated for the gas chromatography/mass spectrometric analysis of chemical warfare agents in water and slurry samples. The chemical warfare agents included four nerve agents and a blister agent. Parameters such as extraction solvent, salt concentration, stirring speed and extraction time were optimised using spiked deionised water samples. The technique provided a linear range of two orders of magnitude, good repeatability (RSDs < 10%, n = 6), good linearity (r2 >or= 0.995) and limits of detection (LODs) in the range of 0.02-0.09 microg l(-1) (S/N = 3) under full scan mode. The optimised technique was also applied to more complex slurry samples and similar precision (RSD < 15%, n = 3) and limits of detection (0.02-0.2 microgl(-1), S/N = 3) were obtained.

摘要

研究了一种基于中空纤维保护的液相微萃取的简单且溶剂用量最少的样品制备技术,用于水和泥浆样品中化学战剂的气相色谱/质谱分析。化学战剂包括四种神经性毒剂和一种糜烂性毒剂。使用加标的去离子水样品对萃取溶剂、盐浓度、搅拌速度和萃取时间等参数进行了优化。该技术提供了两个数量级的线性范围、良好的重复性(相对标准偏差<10%,n = 6)、良好的线性(r2≥0.995)以及在全扫描模式下0.02 - 0.09 μg l(-1)(信噪比 = 3)范围内的检测限。优化后的技术还应用于更复杂的泥浆样品,并获得了类似的精密度(相对标准偏差<15%,n = 3)和检测限(0.02 - 0.2 μg l(-1),信噪比 = 3)。

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