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结合在线萃取和预浓缩与液相色谱-大气压化学电离质谱联用的环境水样中吡啶硫酮锌的改进测定方法。

Improved method for the determination of zinc pyrithione in environmental water samples incorporating on-line extraction and preconcentration coupled with liquid chromatography atmospheric pressure chemical ionisation mass spectrometry.

作者信息

Bones Jonathan, Thomas Kevin V, Paull Brett

机构信息

National Centre for Sensor Research, School of Chemical Sciences, Dublin City University, Glasnevin, Dublin 9, Ireland.

出版信息

J Chromatogr A. 2006 Nov 3;1132(1-2):157-64. doi: 10.1016/j.chroma.2006.07.068. Epub 2006 Aug 24.

Abstract

A method has been developed for the determination of zinc pyrithione (ZnPT) in environmental water samples using monolithic reversed-phase silica columns for rapid on-line large volume solid phase extraction in tandem with on-line matrix removal using sacrificial strong anion exchange (SAX) columns. This is coupled with reversed-phase liquid chromatography with atmospheric pressure chemical ionisation mass spectrometric detection. Limits of detection in spiked river water samples, using a 200 mL preconcentration volume, were determined as 18 ng L(-1), with a limit of quantitation of 62 ng L(-1). The percentage recovery from spiked river water was found to be 72+/-9 (n=3 extractions), whilst overall method precision, following 10 repeat complete analyses was found to be 27% RSD at 1 microg L(-1). Linearity was determined over the concentration range of 0.25-10 microg L(-1) and the calculated regression coefficient was R(2)=0.9802. The method was used to investigate the environmental fate of zinc pyrithione in waters and its partition coefficient between sediment and water phases.

摘要

已开发出一种方法,用于测定环境水样中的吡啶硫酮锌(ZnPT),该方法使用整体式反相硅胶柱进行快速在线大体积固相萃取,并结合使用牺牲性强阴离子交换(SAX)柱进行在线基质去除。该方法与反相液相色谱-大气压化学电离质谱检测联用。在加标河水样品中,使用200 mL预浓缩体积时,检测限为18 ng L⁻¹,定量限为62 ng L⁻¹。加标河水的回收率为72±9(n = 3次萃取),而在1 μg L⁻¹下进行10次重复完整分析后,整体方法精密度为27%相对标准偏差。在0.25 - 10 μg L⁻¹的浓度范围内测定线性,计算得到的回归系数为R² = 0.9802。该方法用于研究吡啶硫酮锌在水中的环境归宿及其在沉积物和水相之间的分配系数。

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