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毛细管电泳法测定饮料样品中的山梨酸盐和苯甲酸盐——通过检查离子迁移率优化方法

Determination of sorbate and benzoate in beverage samples by capillary electrophoresis-Optimization of the method with inspection of ionic mobilities.

作者信息

Costa Ana Carolina O, Perfeito Lisliane da Silva, Tavares Marina F M, Micke Gustavo A

机构信息

Institute of Chemistry, University of Sao Paulo, Sao Paulo, SP, Brazil.

出版信息

J Chromatogr A. 2008 Sep 12;1204(1):123-7. doi: 10.1016/j.chroma.2008.07.075. Epub 2008 Jul 29.

Abstract

The aim of this study was to develop a fast capillary electrophoresis method for the determination of benzoate and sorbate ions in commercial beverages. In the method development the pH and constituents of the background electrolyte were selected using the effective mobility versus pH curves. As the high resolution obtained experimentally for sorbate and benzoate in the studies presented in the literature is not in agreement with that expected from the ionic mobility values published, a procedure to determine these values was carried out. The salicylate ion was used as the internal standard. The background electrolyte was composed of 25 mmol L(-1) tris(hydroxymethyl)aminomethane and 12.5 mmol L(-1) 2-hydroxyisobutyric acid, at pH 8.1. Separation was conducted in a fused-silica capillary (32 cm total length and 8.5 cm effective length, 50 microm I.D.), with short-end injection configuration and direct UV detection at 200 nm for benzoate and salicylate and 254 nm for sorbate ions. The run time was only 28s. A few figures of merit of the proposed method include: good linearity (R(2)>0.999), limit of detection of 0.9 and 0.3 mg L(-1) for benzoate and sorbate, respectively, inter-day precision better than 2.7% (n=9) and recovery in the range 97.9-105%. Beverage samples were prepared by simple dilution with deionized water (1:11, v/v). Concentrations in the range of 197-401 mg L(-1) for benzoate and 28-144 mg L(-1) for sorbate were found in soft drinks and tea.

摘要

本研究的目的是开发一种快速毛细管电泳法,用于测定市售饮料中的苯甲酸根离子和山梨酸根离子。在方法开发过程中,利用有效迁移率与pH曲线来选择背景电解质的pH值和成分。由于文献中所呈现的研究中实验获得的山梨酸根离子和苯甲酸根离子的高分辨率与公布的离子迁移率值所预期的不一致,因此开展了测定这些值的程序。使用水杨酸根离子作为内标。背景电解质由25 mmol L⁻¹三(羟甲基)氨基甲烷和12.5 mmol L⁻¹ 2-羟基异丁酸组成,pH为8.1。在熔融石英毛细管(总长32 cm,有效长度8.5 cm,内径50 µm)中进行分离,采用短端进样配置,对苯甲酸根离子和水杨酸根离子在200 nm处以及山梨酸根离子在254 nm处进行直接紫外检测。运行时间仅为28秒。所提出方法的一些性能指标包括:良好的线性(R²>0.999),苯甲酸根离子和山梨酸根离子的检测限分别为0.9和0.3 mg L⁻¹,日间精密度优于2.7%(n = 9),回收率在97.9 - 105%范围内。饮料样品通过用去离子水简单稀释(1:11,v/v)来制备。在软饮料和茶中发现苯甲酸根离子浓度范围为197 - 401 mg L⁻¹,山梨酸根离子浓度范围为28 - 144 mg L⁻¹。

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