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采用短、细内径柱填充全多孔亚 2μm 颗粒的绿色超快速高效液相色谱法,同时测定地表水和废水中选定的药物类污染物。

Green ultra-fast high-performance liquid chromatographic method using a short narrow-bore column packed with fully porous sub-2 μm particles for the simultaneous determination of selected pharmaceuticals as surface water and wastewater pollutants.

机构信息

Department of Chemistry, University of Waterloo, Waterloo, Ontario, Canada.

出版信息

J Sep Sci. 2013 Jan;36(2):252-61. doi: 10.1002/jssc.201200335. Epub 2012 Dec 10.

DOI:10.1002/jssc.201200335
PMID:23229730
Abstract

Fast separations are very desirable in laboratories that analyze large numbers of samples per day or those needing short turn-around times. Traditional HPLC methods using conventional stationary phases and standard column dimensions require significant amounts of organic solvents and generate large volumes of waste. With growing awareness about the environment, the development of green technologies has been receiving increasing attention. In this work, a very fast green analytical method based on LC-UV using a short narrow bore column packed with fully porous sub-2 μm particles has been developed for simultaneous determination of nine pharmaceuticals in wastewater and surface water. The chromatographic separation was optimized in order to achieve short analysis time and good resolution for all analytes in a single run. All analytes could be separated in 1 min with good resolution. Sample preparation was executed by solid phase extraction using Oasis HLB cartridges. The method developed was validated based on parameters such as linearity, precision, accuracy, detection, and quantification limits. The recovery ranged from 70.9 to 92.5% with SDs not higher than 5.4%, except for acetaminophen and sulphanilamide. LODs ranged from 0.6-2.5 μg/L, while the LOQs were in the range 2-8 μg/L.

摘要

快速分离在每天分析大量样品或需要短周转时间的实验室中非常理想。使用传统固定相和标准柱尺寸的传统 HPLC 方法需要大量有机溶剂,并产生大量废物。随着人们对环境的认识不断提高,绿色技术的发展越来越受到关注。在这项工作中,开发了一种基于 LC-UV 的非常快速的绿色分析方法,该方法使用短而窄的内径柱,柱中填充全多孔亚 2μm 颗粒,用于同时测定废水中和地表水中的九种药物。为了在单次运行中实现所有分析物的短分析时间和良好分辨率,对色谱分离进行了优化。所有分析物都可以在 1 分钟内实现良好的分离度。样品制备是通过固相萃取用 Oasis HLB 小柱进行的。所开发的方法基于线性、精密度、准确度、检测限和定量限等参数进行了验证。回收率在 70.9%至 92.5%之间,SD 不高于 5.4%,除了对乙酰氨基酚和磺胺。LOD 范围在 0.6-2.5μg/L 之间,LOQ 在 2-8μg/L 范围内。

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