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苯甲酸酯和邻苯二甲酸酯衍生物及异构体的毛细管电泳分析

Capillary electrophoretic analysis of the derivatives and isomers of benzoate and phthalate.

作者信息

Wu Chien-Hou, Lo Yu-Shiu, Nian Hung-Chi, Lin Ying-Ying

机构信息

Department of Atomic Science, National Tsing Hua University, 101, Sec. 2, Kuang Fu Road, Hsinchu 30043, Taiwan.

出版信息

J Chromatogr A. 2003 Jun 27;1003(1-2):179-87. doi: 10.1016/s0021-9673(03)00734-9.

Abstract

A capillary electrophoretic method for the analysis of 12 commonly found derivatives and isomers of benzoate and phthalate, including p-toluic acid, p-acetamido and p-hydroxy derivatives of benzoic acid, salicylic acid and its acetyl ester, 2- and 4-isomers of carboxybenzaldehyde, meta-, para-, and ortho-isomers of phthalic acid, and monomethyl terephthalic acid was developed. Capillary electrophoresis (CE) was performed in the free zone electrophoresis mode. Performing CE in 10 mM phosphate buffer, pH 7.0 could separate most of the benzoic acid derivatives except the structural or positional isomers. The positional isomers of phthalic acids could be completely separated with co-addition of alpha- and beta-cyclodextrins. Addition of poly(ethylene glycol) 600 (4%) could further resolve some structural isomers. The CE method developed here is rapid, i.e. complete separation could be achieved in less than 8 min for the nine monoanionic benzoate derivatives and in less than 14 min for the three dianionic phthalate isomers. The new method has good precision and linearity and can be readily applied to real samples for quantitative analysis. It is sensitive and can detect sub-ppm (w/w) level of impurity in real terephthalic samples.

摘要

开发了一种毛细管电泳方法,用于分析12种常见的苯甲酸盐和邻苯二甲酸盐衍生物及异构体,包括对甲苯酸、苯甲酸的对乙酰氨基和对羟基衍生物、水杨酸及其乙酰酯、羧基苯甲醛的2-和4-异构体、邻苯二甲酸的间位、对位和邻位异构体以及对苯二甲酸单甲酯。毛细管电泳(CE)在自由区电泳模式下进行。在pH 7.0的10 mM磷酸盐缓冲液中进行CE可分离大多数苯甲酸衍生物,但结构或位置异构体除外。邻苯二甲酸的位置异构体可通过同时添加α-和β-环糊精完全分离。添加聚乙二醇600(4%)可进一步分离一些结构异构体。这里开发的CE方法速度快,即对于9种单阴离子苯甲酸衍生物,不到8分钟即可实现完全分离,对于3种双阴离子邻苯二甲酸异构体,不到14分钟即可实现完全分离。该新方法具有良好的精密度和线性,可轻松应用于实际样品的定量分析。它灵敏度高,能够检测实际对苯二甲酸样品中低于百万分之一(w/w)水平的杂质。

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