Laboratory for Pharmaceutical Analysis, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, Leuven, Belgium.
J Sep Sci. 2011 Sep;34(18):2448-54. doi: 10.1002/jssc.201100267. Epub 2011 Jul 28.
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.
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)。