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固相萃取结合超高效液相色谱和电喷雾串联质谱法用于高灵敏测定环境水样中的五种碘化X射线造影剂。

Solid-phase extraction coupled with ultra high performance liquid chromatography and electrospray tandem mass spectrometry for the highly sensitive determination of five iodinated X-ray contrast media in environmental water samples.

作者信息

Li Xia, Hu Junjian, Yin Daqiang, Hu Xialin

机构信息

State Key Laboratory of Pollution Control and Resources Reuse, College of Environmental Science and Engineering Tongji University, Shanghai, P.R. China.

出版信息

J Sep Sci. 2015 Jun;38(11):1998-2005. doi: 10.1002/jssc.201401296. Epub 2015 May 7.

Abstract

A highly sensitive method based on solid-phase extraction and ultra high performance liquid chromatography with electrospray tandem mass spectrometry has been developed for simultaneous determination of five iodinated X-ray contrast media in environmental water samples. Various solid-phase extraction cartridges have been evaluated and a combination of LiChrolute EN and ENVI-Carb solid phase extraction cartridges was selected for sample enrichment. The method was comprehensively validated on ground water, tap water, surface water, drinking water, and waste water by the conventional procedures: linearity, method detection limits, accuracy and precision, matrix effects. Good linearity (R(2) > 0.999), low detection limits (0.4-8.1 ng/L), satisfactory recoveries (55.1-109.5%) and precision (0.8-10.0% for intra-day precisions and 0.6-16.5% for inter-day precisions) were obtained for all the target compounds. Iopamidol, iohexol, and diatrizoate in some matrices were affected by matrix effects, which were slightly eased by using the isotope-labeled internal standard. The developed method was successfully applied for real samples collected in Shanghai, China, with detected concentrations up to 2200 ± 200 and 9000 ± 1000 ng/L for iohexol and iopamidol, respectively.

摘要

已开发出一种基于固相萃取和超高效液相色谱-电喷雾串联质谱的高灵敏度方法,用于同时测定环境水样中的五种碘化X射线造影剂。对各种固相萃取柱进行了评估,选择LiChrolute EN和ENVI-Carb固相萃取柱组合用于样品富集。通过线性、方法检出限、准确度和精密度、基质效应等常规程序,对该方法在地下水、自来水、地表水、饮用水和废水中进行了全面验证。所有目标化合物均获得了良好的线性(R(2)>0.999)、低检出限(0.4-8.1 ng/L)、满意的回收率(55.1-109.5%)和精密度(日内精密度为0.8-10.0%,日间精密度为0.6-16.5%)。某些基质中的碘帕醇、碘海醇和泛影酸盐受基质效应影响,使用同位素标记内标可稍有缓解。所开发的方法成功应用于在中国上海采集的实际样品,碘海醇和碘帕醇的检测浓度分别高达2200±200和9000±1000 ng/L。

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