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环糊精修饰胶束电动色谱法分离邻苯二甲酸酯:香水中的定量分析。

Separation of phthalates by cyclodextrin modified micellar electrokinetic chromatography: quantitation in perfumes.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, University of Alcalá, Spain.

出版信息

Anal Chim Acta. 2013 Jun 11;782:67-74. doi: 10.1016/j.aca.2013.03.072. Epub 2013 Apr 22.

Abstract

A new CE method has been developed for the simultaneous separation of a group of parent phthalates. Due to the neutral character of these compounds, the addition of several bile salts as surfactants (sodium cholate (SC), sodium deoxycholate (SDC), sodium taurodeoxycholate (STDC), sodium taurocholate (STC)) to the separation buffer was explored showing the high potential of SDC as pseudostationary phase. However, the resolution of all the phthalates was not achieved when employing only this bile salt as additive, being necessary the addition of neutral cyclodextrins (CD) and organic modifiers to the separation media. The optimized cyclodextrin modified micellar electrokinetic chromatography (CD-MEKC) method consisted of the employ of a background electrolyte (BGE) containing 25 mM β-CD-100 mM SDC in a 100 mM borate buffer (pH 8.5) with a 10% (v/v) of acetonitrile, employing a voltage of 30 kV and a temperature of 25 °C. This separation medium enabled the total resolution of eight compounds and the partial resolution of two of the analytes, di-n-octyl phthalate (DNOP) and diethyl hexyl phthalate (DEHP) (Rs~0.8), in only 12 min. The analytical characteristics of the developed method were studied showing their suitability for the determination of these compounds in commercial perfumes. In all the analyzed perfumes the most common phthalate was diethyl phthalate (DEP) that appeared in ten of the fifteen analyzed products. Also dimethyl phthalate (DMP), diallyl phthalate (DAP), dicyclohexyl phthalate (DCP), and di-n-pentyl phthalate (DNPP) were found in some of the analyzed samples.

摘要

一种新的 CE 方法已被开发用于同时分离一组邻苯二甲酸酯。由于这些化合物的中性性质,在分离缓冲液中添加了几种胆汁盐作为表面活性剂(胆酸钠(SC)、脱氧胆酸钠(SDC)、牛磺脱氧胆酸钠(STDC)、牛磺胆酸钠(STC)),显示出 SDC 作为伪固定相的高潜力。然而,仅使用这种胆汁盐作为添加剂时,未能实现所有邻苯二甲酸酯的分离,需要在分离介质中添加中性环糊精(CD)和有机溶剂。优化的环糊精修饰胶束电动色谱(CD-MEKC)方法包括使用含有 25 mM β-CD-100 mM SDC 的背景电解质(BGE),在 100 mM 硼酸缓冲液(pH 8.5)中添加 10%(v/v)乙腈,施加 30 kV 电压和 25°C 的温度。这种分离介质能够完全分离 8 种化合物,并部分分离两种分析物,即邻苯二甲酸二正辛酯(DNOP)和邻苯二甲酸二乙基己酯(DEHP)(Rs~0.8),仅需 12 分钟。研究了开发方法的分析特性,表明其适用于商业香水这些化合物的测定。在所分析的所有香水中,最常见的邻苯二甲酸酯是邻苯二甲酸二乙酯(DEP),在分析的 15 种产品中的 10 种中都有出现。此外,还在一些分析样品中发现了邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二烯丙酯(DAP)、邻苯二甲酸二环己酯(DCP)和邻苯二甲酸二戊酯(DNPP)。

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