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采用电容耦合非接触电导检测(C4D)的毛细管电泳法同时测定阿替洛尔和阿米洛利。

Simultaneous determination of atenolol and amiloride by capillary electrophoresis with capacitively coupled contactless conductivity detection (C4D).

作者信息

AL Azzam Khaldun M, Aboul-Enein Hassan Y

机构信息

School of Chemical Sciences, Universiti Sains Malaysia, Penang, Malaysia.

出版信息

Methods Mol Biol. 2013;919:67-78. doi: 10.1007/978-1-62703-029-8_7.

Abstract

Capillary electrophoresis coupled with a capacitively coupled contactless conductivity detector (CE-C(4)D) has been employed for the determination of the β-blocker drugs (atenolol and amiloride) in pharmaceutical formulations. 150 mM acetic acid was used as background electrolyte. The influence of several factors (detector excitation voltage and frequency, buffer concentration, applied voltage, capillary temperature, and injection time) was studied. Non-UV absorbing L-valine was used as an internal standard; the analytes were all separated in less than 7 min. The separation was carried out in normal polarity mode at 28 °C, 25 kV, and using hydrodynamic injection (25 s). The separation was effected in a bare fused-silica capillary 75 μm × 52 cm. The CE-C(4)D method was validated with respect to linearity, limit of detection and quantification, accuracy, precision, and selectivity. Calibration curves were linear over the range 5-250 μg mL(-1) for the studied analytes. The relative standard deviations of intra- and inter-day precisions of migration times and corrected peak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneous determination of the β-blocker drugs in different pharmaceutical tablets.

摘要

采用毛细管电泳结合电容耦合非接触式电导检测器(CE-C(4)D)测定药物制剂中的β受体阻滞剂药物(阿替洛尔和阿米洛利)。以150 mM乙酸作为背景电解质。研究了几个因素(检测器激发电压和频率、缓冲液浓度、施加电压、毛细管温度和进样时间)的影响。使用非紫外吸收的L-缬氨酸作为内标;所有分析物在不到7分钟内分离完毕。分离在28℃、25 kV的正常极性模式下进行,采用流体动力学进样(25秒)。在一根75μm×52 cm的裸熔融石英毛细管中进行分离。对CE-C(4)D方法的线性、检测限和定量限、准确度、精密度和选择性进行了验证。所研究分析物的校准曲线在5-250μg mL(-1)范围内呈线性。迁移时间和校正峰面积的日内和日间精密度的相对标准偏差均小于6.0%。该方法具有良好的精密度和准确度,并成功应用于不同药片中β受体阻滞剂药物的同时测定。

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