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毛细管电泳分析阴离子溶质的方法开发策略

Method development strategy for the analysis of anionic solutes by capillary electrophoresis.

作者信息

Colombara R, Tavares M F, Massaro S, Rubim J C

机构信息

Instituto de Química, Universidade de São Paulo, Brazil.

出版信息

J Capillary Electrophor. 1996 May-Jun;3(3):147-53.

PMID:9384747
Abstract

A systematic approach to the development of methodology for the analysis of anionic solutes by capillary electrophoresis (CE) has been implemented. The strategy allows a rapid optimization of the experimental conditions and is based on the following steps: 1) A near optimum pH is chosen by inspection of the effective mobility versus pH curves of the sample components. The optimum pH lies in a region where the differences in the mobilities of all solutes are maximal. 2) An electrolyte system is selected by comparing the effective mobility of the electrolyte with the effective mobility of the primary components of the studied mixture. The appropriate electrolyte has a mobility as similar as possible to the mobility of the major components of the sample. 3) An initial experiment is run with the selected electrolyte system adjusted to the chosen pH and input values for other instrumental variables and electrolyte characteristics. 4) Depending on the degree of resolution obtained in the initial run, two important variables, the applied voltage and the electrolyte concentration, are then tuned in the proper direction, favoring the achievement of the highest resolution at the lowest possible analysis time. The proposed method development strategy was validated experimentally with a mixture of short-chained carboxylic acids and inorganic anions.

摘要

已实施了一种用于毛细管电泳(CE)分析阴离子溶质的系统方法开发策略。该策略基于以下步骤,可实现实验条件的快速优化:1)通过检查样品组分的有效迁移率与pH曲线来选择接近最佳的pH值。最佳pH值位于所有溶质迁移率差异最大的区域。2)通过比较电解质的有效迁移率与所研究混合物主要成分的有效迁移率来选择电解质系统。合适的电解质迁移率应尽可能与样品主要成分的迁移率相似。3)使用选定的电解质系统,将其调整到选定的pH值,并设置其他仪器变量和电解质特性的输入值,进行初始实验。4)根据初始运行中获得的分离度,然后在适当方向上调整两个重要变量,即施加电压和电解质浓度,以利于在尽可能短的分析时间内实现最高分离度。所提出的方法开发策略通过短链羧酸和无机阴离子混合物进行了实验验证。

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