Department of Chemistry, College of Science, King Faisal University, Al-Ahsa 31982, Saudi Arabia.
Department of Chemistry, College of Science, King Khalid University, Abha 62529, Saudi Arabia.
Molecules. 2023 Jan 25;28(3):1184. doi: 10.3390/molecules28031184.
A capillary zone electrophoretic (CZE) method was developed, validated, and applied for the assay of metformin (MET) and pioglitazone (PIO) in pharmaceutical formulations. The optimum running buffer composition was found to be 75 mmol/L phosphate buffer containing 30% acetonitrile (ACN) at pH 4.0. The optimum instrumental conditions were found to be injection time, 10 s; applied voltage, 25 kV; hydrodynamic injection pressure, 0.5 psi for 10 s, capillary temperature, 25 °C; and the detection wavelength, 210 nm. The quantifications were calculated based on the ratio of the peak areas of analytes to atenolol as an internal standard. The CZE method was validated in terms of accuracy (98.21-104.81%), intra- and inter-day precision of migration time and peak area (relative standard deviation ≤ 5%), linearity (correlation coefficients ≥ 0.9985), limit of detection (≤0.277 μg/mL), and limit of quantitation (≤0.315 μg/mL). The proposed method was applied for the analysis of PIO and MET both individually and in a combined dosage tablet formulation. All electrophoretic parameters were calculated and evaluated. A previously reported high-performance liquid chromatographic (HPLC) method was also applied to the same samples. A comprehensive comparison was then carried out for the analytical features of both methods CZE and HPLC. Comparable results were obtained with the advantage of reagent consumption and separation efficiency of CZE over HPLC and shorter analysis time by HPLC compared with CZE.
建立并验证了毛细管区带电泳(CZE)法,用于测定药物制剂中的二甲双胍(MET)和吡格列酮(PIO)。结果表明,最优运行缓冲液组成为 75mmol/L 磷酸盐缓冲液,内含 30%乙腈(ACN),pH 值为 4.0。最优仪器条件为:进样时间 10s,施加电压 25kV,液压进样压力 0.5psi 持续 10s,毛细管温度 25°C,检测波长 210nm。定量计算基于分析物峰面积与作为内标物的阿替洛尔的比值。该 CZE 方法在准确度(98.21%-104.81%)、日内和日间迁移时间和峰面积精密度(相对标准偏差≤5%)、线性(相关系数≥0.9985)、检测限(≤0.277μg/mL)和定量限(≤0.315μg/mL)方面进行了验证。该方法应用于 PIO 和 MET 的单独分析和复方片剂制剂分析。计算并评估了所有电泳参数。还应用了先前报道的高效液相色谱(HPLC)方法对相同的样品进行分析。然后对 CZE 和 HPLC 两种方法的分析特性进行了全面比较。两种方法的结果具有可比性,CZE 法在试剂消耗和分离效率方面优于 HPLC 法,HPLC 法在分析时间方面优于 CZE 法。