采用暂态移动化学反应界面法在毛细管电泳中测定富马酸和马来酸。

Determination of fumaric and maleic acids with stacking analytes by transient moving chemical reaction boundary method in capillary electrophoresis.

机构信息

College of Chemistry and Chemical Engineering, Graduate University of Chinese Academy of Sciences, 19A YuQuan Road, Beijing 100049, China.

出版信息

J Chromatogr A. 2011 Jun 17;1218(24):3816-21. doi: 10.1016/j.chroma.2011.04.047. Epub 2011 Apr 27.

DOI:10.1016/j.chroma.2011.04.047

PMID:21565348

Abstract

The paper presents an on-line transient moving chemical reaction boundary (MCRB) method for simply but efficiently stacking analytes in capillary electrophoresis (CE). The CE technique was developed for a rapid determination of fumaric and maleic acid. Based on the theory of MCRB, Effects of several important factors such as the pH and concentration of running buffer and the conditions of stacking analytes were investigated to acquire the optimum conditions. The optimized separations were carried out in a 20 mmol/L sulphate neutralized with ethylenediamine to pH 6.0 electrolytes using a capillary coated with poly (diallyldimethylammonium chloride) and direct UV detection at 214 nm. The optimized preconcentrations were carried out in 50 mmol/L borax (pH 9.0). The calibration curves were linear in the concentration range of 1.0×10⁻⁷-1.0×10⁻⁴ mol/L and 5.0×10⁻⁷-1.0×10⁻⁴ mol/L for fumaric and maleic acid with correlation coefficients higher than 0.9991. The detection limits were 5.34×10⁻⁸ mol/L for fumaric acid and 1.92×10⁻⁷ mol/L for maleic acid. This method was applied for determination of fumaric acid in apple juice and of fumaric and maleic acid in dl-malic, the recovery tests established for real samples were within the range 95-105%. This work provided a valid and simple approach to detect fumaric and maleic acid.

摘要

本文提出了一种在线瞬态移动化学反应边界（MCRB）方法，用于在毛细管电泳（CE）中简单但有效地堆积分析物。CE 技术是为快速测定富马酸和马来酸而开发的。基于 MCRB 理论，考察了几种重要因素，如运行缓冲液的 pH 值和浓度以及堆积分析物的条件，以获得最佳条件。在 20 mmol/L 硫酸盐中用乙二胺中和至 pH 6.0 的电解质中进行优化分离，使用涂有聚（二烯丙基二甲基氯化铵）的毛细管，并在 214nm 处直接紫外检测。在 50 mmol/L 硼砂（pH 9.0）中进行最佳预浓缩。校准曲线在线性范围内为 1.0×10⁻⁷-1.0×10⁻⁴ mol/L 和 5.0×10⁻⁷-1.0×10⁻⁴ mol/L，富马酸和马来酸的相关系数均高于 0.9991。检测限分别为富马酸 5.34×10⁻⁸ mol/L 和马来酸 1.92×10⁻⁷ mol/L。该方法用于测定苹果汁中的富马酸以及 dl-苹果酸中的富马酸和马来酸，对实际样品的回收率试验在 95-105%范围内。这项工作为检测富马酸和马来酸提供了一种有效而简单的方法。