Alzoman Nourah Z, Sultan Maha A, Maher Hadir M, Al-Shehri Mona M, Olah Ileana V
King Saud University, College of Pharmacy, Department of Pharmaceutical Chemistry, Riyadh 11495, PO Box 22452, Saudi Arabia.
J AOAC Int. 2013 Sep-Oct;96(5):951-9. doi: 10.5740/jaoacint.11-245.
A novel, fast, sensitive, and specific capillary electrophoresis (CE) technique coupled to a diode array detector has been developed for the separation and simultaneous determination of carvedilol (CRV) and hydrochlorothiazide (HCT) in two combination formulations. The proposed method utilized a fused silica capillary (55 cm x75 microm id) and the background electrolyte solution phosphate buffer (12.5 mM, pH 7.4)-methanol (95+5, v/v). The separation was achieved at 30 kV applied voltage and 24 degree C. Atorvastatin (80 microg/mL) was chosen as the internal standard. The described method was linear over the range of 1-200 and 0.2-150 microg/mL for CRV and HCT, respectively. Intraday and interday RSD (n = 6) was < or =1.4%. The LOD values of CRV and HCT were 0.26 and 0.07 microg/mL, respectively. The validated CE method was successfully applied to the analysis of two commercial tablet dosage forms. Forced degradation studies were performed on bulk samples of the two drugs using thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Degradation products produced as a result of stress studies did not interfere with the determination of CRV and HCT; the assay could, therefore, be considered stability-indicating.
已开发出一种新颖、快速、灵敏且特异的毛细管电泳（CE）技术，该技术与二极管阵列检测器联用，用于分离并同时测定两种复方制剂中的卡维地洛（CRV）和氢氯噻嗪（HCT）。所提出的方法采用熔融石英毛细管（55 cm×75 μm内径），背景电解质溶液为磷酸盐缓冲液（12.5 mM，pH 7.4）-甲醇（95 + 5，v/v）。在30 kV施加电压和24℃条件下实现分离。选用阿托伐他汀（80 μg/mL）作为内标。所描述的方法对于CRV和HCT分别在1 - 200 μg/mL和0.2 - 150 μg/mL范围内呈线性。日内和日间相对标准偏差（n = 6）≤1.4%。CRV和HCT的检测限分别为0.26和0.07 μg/mL。经过验证的CE方法成功应用于两种市售片剂剂型的分析。使用热、光解、水解和氧化应激条件对两种药物的原料药样品进行强制降解研究，并采用所提出的方法对受应激样品进行分析。应激研究产生的降解产物不干扰CRV和HCT的测定；因此，该测定法可被视为稳定性指示方法。
