Alnajjar Ahmed O, Idris Abubakr M, Attimarad Mahesh V, Aldughaish Adnan M, Elgorashe Rafea E E
Department of Chemistry, College of Science, King Faisal University, Hofuf, Saudi Arabia.
J Chromatogr Sci. 2013 Jan;51(1):92-7. doi: 10.1093/chromsci/bms107. Epub 2012 Jun 28.
The current manuscript reports the first capillary electrophoresis method for the separation and quantification of metoprolol (MET) and hydrochlorothiazide (HCT) in their combined dosage form. MET and HCT were detected at 240 and 214 nm, respectively, using a photodiode array detector. The univariate approach was used for optimizing voltage, injection time and capillary temperature. The factorial design with response surface plots, as a multivariate approach, was used to study the effect of buffer concentration and pH on resolution, peak area and migration time. The optimum conditions were 50 mmol/L phosphate at pH 9.5, injection time 10.0 s, voltage 25 kV and capillary temperature 25°C. The method was linear in the range of 2.5-250 µg/mL for both drugs with correlation coefficients above 0.9997. Additionally, acceptable recovery of the contents of MET and HCT in their formulations (96.0-100.3%) with acceptable precision (1.38-2.60 %) were achieved. Moreover, the limits of detection of MET and HCT were 0.02 and 0.01 µg/mL, respectively, which were suitable for pharmaceutical analysis.
当前的手稿报道了首个用于分离和定量美托洛尔（MET）和氢氯噻嗪（HCT）复方制剂的毛细管电泳方法。使用光电二极管阵列检测器，分别在240 nm和214 nm处检测到MET和HCT。采用单变量方法优化电压、进样时间和毛细管温度。作为多变量方法，采用带有响应面图的析因设计来研究缓冲液浓度和pH对分离度、峰面积和迁移时间的影响。最佳条件为pH 9.5的50 mmol/L磷酸盐、进样时间10.0 s、电压25 kV和毛细管温度25°C。该方法对两种药物在2.5 - 250 µg/mL范围内呈线性，相关系数高于0.9997。此外，制剂中美托洛尔和氢氯噻嗪含量的回收率在可接受范围内（96.0 - 100.3%），精密度也可接受（1.38 - 2.60%）。而且，美托洛尔和氢氯噻嗪的检测限分别为0.02和0.01 µg/mL，适用于药物分析。
