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建立并验证了一种以毛细管电泳-电容耦合非接触式电导检测(CE-C(4) D)为检测手段的方法,用于分析阿米卡星及其相关物质。

Development and validation of a capillary electrophoresis method with capacitively coupled contactless conductivity detection (CE-C(4) D) for the analysis of amikacin and its related substances.

机构信息

Laboratory for Pharmaceutical Analysis, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, Leuven, Belgium.

出版信息

Electrophoresis. 2012 Sep;33(17):2777-82. doi: 10.1002/elps.201100688.

DOI:10.1002/elps.201100688
PMID:22965725
Abstract

Amikacin is a semisynthetic aminoglycoside antibiotic derived from kanamycin A that lacks a strong UV absorbing chromophore or fluorophore. Due to the physicochemical properties of amikacin and its related substances, CE in combination with capacitively coupled contactless conductivity detection (CE-C(4) D) was chosen. The optimized separation method uses a BGE composed of 20 mM MES adjusted to pH 6.6 by l-histidine and 0.3 mM CTAB that was added as flow modifier in a concentration below the CMC. Ammonium acetate 20 mg.L(-1) was used as internal standard. 30 kV was applied in reverse polarity on a fused silica capillary (73/48 cm; 75 μm id). The optimized separation was obtained in less than 6 min with good linearity (R(2) = 0.9996) for amikacin base. It shows a good precision expressed as RSD on relative peak areas equal to 0.1 and 0.7% for intraday and interday, respectively. The LOD and LOQ are 0.5 mg.L(-1) and 1.7 mg.L(-1) , respectively.

摘要

阿米卡星是一种从卡那霉素 A 衍生而来的半合成氨基糖苷类抗生素,缺乏强的紫外吸收生色团或荧光团。由于阿米卡星及其相关物质的物理化学性质,选择了 CE 与电容耦合非接触式电导检测(CE-C(4) D)相结合。优化的分离方法使用由 20 mM MES 组成的 BGE,通过 l-组氨酸调节 pH 值至 6.6,并添加低于 CMC 的浓度作为流动改性剂的 CTAB。20 mg.L(-1)的乙酸铵用作内标。在熔融石英毛细管(73/48 cm;75 μm id)上施加 30 kV 的反向极性。在不到 6 分钟的时间内即可获得良好的线性(阿米卡星碱的 R(2) = 0.9996)。分别以相对峰面积的 RSD 表示,日内和日间的精密度均良好,分别为 0.1%和 0.7%。LOD 和 LOQ 分别为 0.5 mg.L(-1)和 1.7 mg.L(-1)。

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