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在毛细管电泳(CE)中,作为一种替代检测模式的电容耦合非接触式电导检测法,用于硫酸卡那霉素及其有关物质的分析。

Capacitively coupled contactless conductivity detection as an alternative detection mode in CE for the analysis of kanamycin sulphate and its related substances.

机构信息

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

出版信息

J Sep Sci. 2011 Sep;34(18):2448-54. doi: 10.1002/jssc.201100267. Epub 2011 Jul 28.

Abstract

A method was developed to determine simultaneously kanamycin, its related substances and sulphate in kanamycin sulphate using capacitively coupled contactless conductivity detection. Kanamycin is an aminoglycoside antibiotic that lacks a strong UV-absorbing chromophore. Due to its physicochemical properties, CE in combination with capacitively coupled contactless conductivity detection was chosen. The separation method uses a BGE composed of 40 mM 2-(N-morpholino)ethanesulphonic acid monohydrate and 40 mM L-histidine, pH 6.35. A 0.6 mM N-cetyltrimethyl ammonium bromide (CTAB) solution was added as electroosmotic flow modifier in a concentration below the critical micellar concentration (CMC). Ammonium acetate 50 mg/L was used as internal standard. In total, 30 kV was applied in reverse polarity on a fused-silica capillary (65/41 cm; 75 μm id). The optimized separation was obtained in less than 6 min with good linearity (R(2)=0.9999) for kanamycin. It shows a good precision expressed as RSD on the relative peak areas equal to 0.3 and 1.1% for intra-day and inter-day precision, respectively. The LOD and LOQ are 0.7 and 2.3 mg/L, respectively. Similarly, for sulphate, a good linearity (R(2)=0.9996) and precision (RSD 0.4 and 0.6% for intra-day and inter-day, respectively) were obtained.

摘要

建立了同时测定硫酸卡那霉素中卡那霉素、有关物质和硫酸盐的方法。卡那霉素是一种氨基糖苷类抗生素,缺乏强的紫外吸收生色团。由于其理化性质,选择了 CE 与电容耦合非接触式电导检测相结合的方法。该分离方法使用由 40 mM 2-(N-吗啉基)乙磺酸一水合物和 40 mM L-组氨酸组成的 BGE,pH 值为 6.35。在低于临界胶束浓度(CMC)的浓度下,加入 0.6 mM N-十六烷基三甲基溴化铵(CTAB)溶液作为电渗流改性剂。使用 50 mg/L 乙酸铵作为内标。在反向极性下,总共施加 30 kV 于熔融硅毛细管(65/41 cm;75 μm id)上。在不到 6 分钟的时间内获得了优化的分离,卡那霉素的线性度良好(R²=0.9999)。它显示出良好的精密度,表现在相对峰面积的 RSD 分别为 0.3%和 1.1%,分别为日内和日间精密度。LOD 和 LOQ 分别为 0.7 和 2.3 mg/L。同样,硫酸盐也获得了良好的线性度(R²=0.9996)和精密度(RSD 分别为 0.4%和 0.6%,分别为日内和日间)。

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