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在3-巯基丙酸存在下,用邻苯二甲醛进行毛细管内衍生化,通过紫外检测的毛细管电泳同时测定食品样品中的谷氨酸钠、苯甲酸和山梨酸。

In-capillary derivatization with o-phthalaldehyde in the presence of 3-mercaptopropionic acid for the simultaneous determination of monosodium glutamate, benzoic acid, and sorbic acid in food samples via capillary electrophoresis with ultraviolet detection.

作者信息

Aung Hnin-Pwint, Pyell Ute

机构信息

Department of Chemical Science, Faculty of Science, Universiti Tunku Abdul Rahman, 31900 Kampar, Malaysia; Centre for Bio-Diversity Research, Universiti Tunku Abdul Rahman, 31900 Kampar, Malaysia.

Department of Chemistry, University of Marburg, Hans-Meerwein-Strasse, D-35032 Marburg, Germany.

出版信息

J Chromatogr A. 2016 Jun 3;1449:156-65. doi: 10.1016/j.chroma.2016.04.033. Epub 2016 Apr 20.

DOI:10.1016/j.chroma.2016.04.033
PMID:27156753
Abstract

For the rapid simultaneous determination of monosodium glutamate (MSG), benzoic acid (BA), and sorbic acid (SA) in canned food and other processed food samples, we developed a method that combines in-capillary derivatization with separation by capillary electrophoresis. This method employs the rapid derivatization of MSG with o-phthalaldehyde (OPA) in the presence of 3-mercaptopropionic acid (3-MPA) and enables the detection of the resulting OPA-MSG derivative and of non-derivatized BA and SA at 230nm. The composition of the background electrolyte and the parameters of derivatization and separation are as follows: 25mM borax containing 5mM OPA and 6mM 3-MPA, separation voltage 25mV, injection at 30mbar for 20s, and column temperature 25°C. Because of the high reaction rate and suitably adapted effective electrophoretic mobilities, band broadening due to the derivatization reaction at the start of the separation process is kept to a minimum. The optimized method is validated with respect to LOD, LOQ, linearity, recovery, and precision. This method can be applied to real samples such as soy, fish, oyster and sweet and sour chili sauces after application of appropriate clean-up steps. Mechanisms of zone broadening and zone focusing are discussed showing the validity of the employed theoretical approach regarding the dependence of the peak shape for OPA-MSG on the concentration of MSG in the sample.

摘要

为了快速同时测定罐头食品和其他加工食品样品中的味精(MSG)、苯甲酸(BA)和山梨酸(SA),我们开发了一种将毛细管内衍生化与毛细管电泳分离相结合的方法。该方法利用邻苯二甲醛(OPA)在3-巯基丙酸(3-MPA)存在下对味精进行快速衍生化,并能在230nm处检测生成的OPA-MSG衍生物以及未衍生化的BA和SA。背景电解质的组成以及衍生化和分离参数如下:含5mM OPA和6mM 3-MPA的25mM硼砂,分离电压25mV,30mbar进样20s,柱温25°C。由于反应速率高且有效电泳迁移率适配得当,分离过程开始时衍生化反应导致的谱带展宽被降至最低。该优化方法在检测限、定量限、线性、回收率和精密度方面得到了验证。经过适当的净化步骤后,该方法可应用于大豆、鱼类、牡蛎以及酸甜辣椒酱等实际样品。文中讨论了区带展宽和区带聚焦的机制,表明所采用的关于OPA-MSG峰形依赖于样品中味精浓度的理论方法的有效性。

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