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采用非接触式电导检测的毛细管区带电泳法快速测定药品和营养保健品中的氨基葡萄糖。

Fast assay of glucosamine in pharmaceuticals and nutraceuticals by capillary zone electrophoresis with contactless conductivity detection.

作者信息

Jác Pavel, Los Petr, Spácil Zdenek, Pospísilová Marie, Polásek Miroslav

机构信息

Department of Analytical Chemistry, Charles University, Heyrovského, Hradec Králové, Czech Republic.

出版信息

Electrophoresis. 2008 Sep;29(17):3511-8. doi: 10.1002/elps.200800068.

Abstract

A novel capillary electrophoresis (CE) method with contactless conductivity detection suitable for the determination of glucosamine (GlAm) and K(+) in pharmaceuticals was devised. Under the optimum conditions (aqueous 30 mM acetate buffer of pH 5.2 as the background electrolyte; voltage 30 kV; 25 degrees C), GlAm (migrating as glucosaminium cation) was well separated from K(+) that could occur in the dosage forms as excipient. The CE analysis was performed in fused-silica capillaries (50 microm i.d., 75 cm total length, 27 cm to detector) and the separation took <3 min. The calibration graphs were linear for both GlAm (100-300 microg/mL; r(2)=0.997) and K(+) (15-75 microg/mL; r(2)=0.997) when using ethanolamine (100 microg/mL) as the internal standard. The LOD values (S/N=3) were 9.3 microg/mL for GlAm and 2.9 microg/mL for K(+). The method was applied to the assay of GlAm content in various dosage forms. Intermediate precision evaluated by determining the content of GlAm in a single formulation on 3 consecutive days was characterized by RSD 2.35% (n=15). Acceptable accuracy of the CE method was confirmed by the added/found GlAm recovery experiments (recoveries 94.6-103.3%) and by statistical comparison of the results attained by the proposed CE and a reference HPLC method.

摘要

设计了一种采用非接触式电导检测的新型毛细管电泳(CE)方法,适用于测定药物中的氨基葡萄糖(GlAm)和钾离子(K⁺)。在最佳条件下(以pH 5.2的30 mM醋酸盐水溶液作为背景电解质;电压30 kV;25℃),GlAm(以葡糖胺阳离子形式迁移)与可能作为辅料存在于剂型中的K⁺得到了很好的分离。CE分析在熔融石英毛细管(内径50μm,总长度75 cm,至检测器的长度27 cm)中进行,分离时间小于3分钟。当使用乙醇胺(100μg/mL)作为内标时,GlAm(100 - 300μg/mL;r² = 0.997)和K⁺(15 - 75μg/mL;r² = 0.997)的校准曲线均呈线性。GlAm的检测限(S/N = 3)为9.3μg/mL,K⁺的检测限为2.9μg/mL。该方法应用于各种剂型中GlAm含量的测定。通过连续3天测定单一制剂中GlAm的含量来评估中间精密度,其相对标准偏差(RSD)为2.35%(n = 15)。通过加样/回收率实验(回收率94.6 - 103.3%)以及将所提出的CE方法与参考HPLC方法所得结果进行统计比较,证实了CE方法具有可接受的准确度。

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