Barden A T, Piccoli B L, Volpato N M, Schapoval E E S, Steppe M
Pharmazie. 2014 Feb;69(2):86-91.
A stability-indicating capillary zone electrophoresis (CZE) method was validated for the determination of vildagliptin (VLG) in pharmaceutical dosage forms using ranitidine hydrochloride (RH) as internal standard. The CZE method was carried out in a fused silica capillary (64.5 cm total length and 56.0 cm effective length, 50 microm i.d.) by applying a potential of 25 kV (positive polarity), hydrodynamic injection by 50 mbar for 5 s and the temperature of the capillary cartridge was 25 degreesC. The selected background electrolyte (BGE) consisted of 25 mM potassium phosphate (pH 8.0) with UV/PDA detection at 207 nm. The electrophoretic separation was obtained within 6 min and was linear in the range of 50-200 microg/mL (r= 0.9994). The specificity and the stability-indicating capability were demonstrated through degradation studies, which also showed that there was no interference of the formulation excipients. The method was validated in accordance to ICH guidelines acceptance criteria for specificity, linearity, precision, accuracy, robustness and system suitability. The proposed method was compared with HPLC method previously validated for this drug, and statistical analysis showed no significant difference between the methods.
建立了一种稳定性指示毛细管区带电泳（CZE）法，以盐酸雷尼替丁（RH）为内标，用于测定药物剂型中的维格列汀（VLG）。CZE法在熔融石英毛细管（总长64.5 cm，有效长度56.0 cm，内径50 µm）中进行，施加25 kV（正极性）的电压，以50 mbar的压力进行5 s的流体动力学进样，毛细管柱温度为25℃。选用的背景电解质（BGE）为25 mM磷酸钾（pH 8.0），在207 nm处进行紫外/光电二极管阵列检测。电泳分离在6分钟内完成，在50-200 μg/mL范围内呈线性（r = 0.9994）。通过降解研究证明了该方法的特异性和稳定性指示能力，研究还表明制剂辅料无干扰。该方法按照ICH指南中关于特异性、线性、精密度、准确度、稳健性和系统适用性的接受标准进行了验证。将所提出的方法与先前针对该药物验证的HPLC方法进行比较，统计分析表明两种方法之间无显著差异。
