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毛细管电泳-电化学检测法测定黄芪及其制剂中的活性成分

[Determination of active components in Radix astragali and its medicinal preparations by capillary electrophoresis with electrochemical detection].

作者信息

Jin Shuping, Li Ping, Dong Shuqing, Wang Qingjiang, Fang Yuzhi

机构信息

Department of Chemistry, East China Normal University, Shanghai 200062, China.

出版信息

Se Pu. 2009 Mar;27(2):229-32.

Abstract

A simple, fast, and reliable method based on capillary electrophoresis with electrochemical detection (CE-ED) was developed for the separation and determination of rutin, ferulic acid, vanillic acid, chlorogenic acid, quercetin and caffeic acid in Radix Astragali and its medicinal preparations. The effects of several important factors, such as detection potential, pH, running buffer concentration, separation voltage and injection time, were investigated to acquire the optimum conditions. Under the optimum conditions, the analytes could be separated within 17 min in a 75 cm length capillary at a separation voltage of 18 kV in a 10 mmol/L borate buffer (pH 8.2). A 300 microm diameter carbon disk electrode generated a good response at +0.95 V (vs. saturated calomel electrode (SCE)) for all analytes. The relationship between peak currents and analyte concentrations was linear over about three orders of magnitude with detection limits (S/N = 3) ranging from 78 microg/L to 110 microg/L for all analytes. The average recoveries were 96.0%-103.0% with the relative standard deviations of 1.9%-3.6% (n=3). This method has been successfully used for the determination of these analytes in real samples, and the assay results were satisfactory.

摘要

建立了一种基于毛细管电泳 - 电化学检测(CE - ED)的简单、快速且可靠的方法,用于分离和测定黄芪及其药用制剂中的芦丁、阿魏酸、香草酸、绿原酸、槲皮素和咖啡酸。研究了检测电位、pH值、运行缓冲液浓度、分离电压和进样时间等几个重要因素的影响,以获得最佳条件。在最佳条件下,在10 mmol/L硼酸盐缓冲液(pH 8.2)中,于75 cm长的毛细管中,在18 kV的分离电压下,17分钟内可分离分析物。直径为300微米的碳盘电极对所有分析物在 +0.95 V(相对于饱和甘汞电极(SCE))时产生良好响应。峰电流与分析物浓度之间的关系在大约三个数量级内呈线性,所有分析物的检测限(S/N = 3)为78 μg/L至110 μg/L。平均回收率为96.0% - 103.0%,相对标准偏差为1.9% - 3.6%(n = 3)。该方法已成功用于实际样品中这些分析物的测定,测定结果令人满意。

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