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使用全多孔亚 2μm 柱在高温下同时测定水样中选定磺胺类药物的快速超高效液相色谱方法的优化与验证

Optimization and validation of a fast ultrahigh-pressure liquid chromatographic method for simultaneous determination of selected sulphonamides in water samples using a fully porous sub-2 μm column at elevated temperature.

作者信息

Shaaban Heba, Górecki Tadeusz

机构信息

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

出版信息

J Sep Sci. 2012 Jan;35(2):216-24. doi: 10.1002/jssc.201100754. Epub 2011 Dec 12.

DOI:10.1002/jssc.201100754
PMID:22162242
Abstract

High temperature in HPLC is considered a valuable tool helping to overcome the increase in the column backpressure when using small packing particles such as sub-2 μm, as it allows reduction in the mobile-phase viscosity. In this study, a fast analytical method based on HPLC-UV was developed using a sub-2 μm column at elevated temperature for the simultaneous determination of nine sulphonamides. Owing to the lower viscosity of the mobile phase, the separation could be achieved in 3 min at 60°C for all analytes. The effect of temperature, the organic modifier percentage and the flow rate on the retention time was studied. The method developed was used for the determination of selected sulphonamides in surface and wastewater samples. Sample preparation was carried out by solid-phase extraction on Oasis HLB cartridges. The method developed was validated based on the linearity, precision, accuracy, detection and quantification limits. The recovery ranged from 70.6 to 96 % with standard deviations not higher than 4.7%, except for sulphanilamide. Limits of detection ranged from 1 to 10 μg/L after optimization of all analytical steps. This method has the highest performance in terms of analytical speed compared with other published HPLC-UV methods for the determination of sulphonamides in water.

摘要

在高效液相色谱(HPLC)中,高温被视为一种有价值的工具,有助于克服使用小粒径填料(如亚2μm)时柱背压的增加,因为它能降低流动相的粘度。在本研究中,开发了一种基于HPLC-紫外检测(HPLC-UV)的快速分析方法,该方法使用亚2μm色谱柱在高温下同时测定9种磺胺类药物。由于流动相粘度较低,所有分析物在60℃下3分钟内即可实现分离。研究了温度、有机改性剂百分比和流速对保留时间的影响。所开发的方法用于测定地表水和废水样品中的选定磺胺类药物。样品制备通过在Oasis HLB柱上进行固相萃取来完成。所开发的方法根据线性、精密度、准确度、检测限和定量限进行了验证。除磺胺外,回收率在70.6%至96%之间,标准偏差不高于4.7%。在优化所有分析步骤后,检测限范围为1至10μg/L。与其他已发表的用于测定水中磺胺类药物的HPLC-UV方法相比,该方法在分析速度方面具有最高的性能。

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