Yardimci Ceren, Ozaltin Nuran
Department of Analytical Chemistry, Faculty of Pharmacy, Hacettepe University, 06100, Sihhiye, Ankara, Turkey.
J Chromatogr Sci. 2010 Feb;48(2):95-9. doi: 10.1093/chromsci/48.2.95.
A micellar electrokinetic capillary chromatography method was developed and validated for the simultaneous determination of ezetimibe and simvastatin in pharmaceutical preparations. The influence of buffer concentration, buffer pH, sodium dodecyl sulphate (SDS) concentration, organic modifier, capillary temperature, applied voltage, and injection time was investigated, and the method validation studies were performed. The optimum separation for these analytes was achieved in less than 10 min at 30 degrees C with a fused-silica capillary column (56 cm x 50 microm i.d.) and a 25mM borate buffer at pH 9.0 containing 25mM SDS and 10% (v/v) acetonitrile. The samples were injected hydrodynamically for 3 s at 50 mbar, and the applied voltage was +30.0 kV. Detection wavelength was set at 238 nm. Diflunisal was used as internal standard. The method was suitably validated with respect to stability, specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness. The limits of detection and quantification were 1.0 and 2.0 microg/mL for both ezetimibe and simvastatin, respectively. The method developed was successfully applied to the simultaneous determination of ezetimibe and simvastatin in pharmaceutical preparations.
建立并验证了一种胶束电动毛细管色谱法，用于同时测定药物制剂中的依折麦布和辛伐他汀。研究了缓冲液浓度、缓冲液pH值、十二烷基硫酸钠（SDS）浓度、有机改性剂、毛细管温度、施加电压和进样时间的影响，并进行了方法验证研究。在30℃下，使用熔融石英毛细管柱（56 cm×50μm内径）和pH 9.0的25 mM硼酸盐缓冲液（含25 mM SDS和10%（v/v）乙腈），在不到10分钟内实现了这些分析物的最佳分离。样品在50 mbar下进行3 s的流体动力学进样，施加电压为+30.0 kV。检测波长设定为238 nm。双氟尼酸用作内标。该方法在稳定性、特异性、线性、检测限和定量限、准确度、精密度和稳健性方面得到了适当验证。依折麦布和辛伐他汀的检测限和定量限分别为1.0和2.0μg/mL。所建立的方法成功应用于药物制剂中依折麦布和辛伐他汀的同时测定。
