El-Zaher Asmaa A, Elkady Ehab F, Elwy Hanan M, Saleh Mahmoud A
Cairo University, Faculty of Pharmacy, Pharmaceutical Chemistry Department, Kasr El-Aini St, Cairo 11562, Egypt.
National Organization for Drug Control and Research (NODCAR), Giza 35521, Egypt.
J AOAC Int. 2016 Jul;99(4):957-963. doi: 10.5740/jaoacint.15-0291. Epub 2016 May 20.
A rapid, simple, and precise RPLC method was developed for the simultaneous determination of the widely used oral antidiabetic, metformin hydrochloride (MTF), with some commonly coadministered oral antidiabetics from different pharmacological classes-glipizide (GPZ), pioglitazone hydrochloride (PGZ), glimepiride (GLM), and repaglinide (RPG)-in bulk, laboratory-prepared mixtures and pharmaceutical formulations in the presence of metformin-reported impurity [1-cyanoguanidine (CNG)]. Chromatographic separation was achieved using isocratic elution mode with a mobile phase of acetonitrile: 0.02 M potassium dihydrogen phosphate (pH 3.17; 50-50, v/v) flowing through a CN Phenomenex column (Phenosphere Next, 250 × 4.6 mm, 5 μm) at a rate of 1.5 mL/min at ambient temperature. UV detection was carried out at 220 nm. The method was validated according to International Conference on Harmonization guidelines. Linearity, accuracy, and precision were satisfactory for concentration ranges: 0.175-350 μg/mL for MTF, 0.0525-105 μg/mL for GPZ, 0.125-250 μg/mL for PGZ, and 0.05-100 μg/mL for GLM and RPG. Correlation coefficients were >0.99 for all analytes. LOQs were 0.009 μg/mL for MTF, 0.009 μg/mL for GPZ, 0.04 μg/mL for GLM, 0.124 μg/mL for PGZ, and 0.044 μg/mL for RPG. The developed method is specific, accurate, and suitable for the QC and routine analysis of the cited drugs in their pharmaceutical products.
开发了一种快速、简单且精确的反相高效液相色谱（RPLC）方法，用于同时测定广泛使用的口服抗糖尿病药物盐酸二甲双胍（MTF）以及一些来自不同药理类别的常用联合口服抗糖尿病药物——格列吡嗪（GPZ）、盐酸吡格列酮（PGZ）、格列美脲（GLM）和瑞格列奈（RPG），这些药物以原料药、实验室制备的混合物以及存在二甲双胍报告杂质[1-氰基胍（CNG）]的药物制剂形式存在。采用等度洗脱模式，以乙腈：0.02 M磷酸二氢钾（pH 3.17；50-50，v/v）为流动相，在室温下以1.5 mL/min的流速流经CN Phenomenex柱（Phenosphere Next，250×4.6 mm，5μm）进行色谱分离。在220 nm处进行紫外检测。该方法根据国际协调会议指南进行了验证。对于以下浓度范围，线性、准确度和精密度均令人满意：MTF为0.175-350μg/mL，GPZ为0.0525-105μg/mL，PGZ为0.125-250μg/mL，GLM和RPG为0.05-100μg/mL。所有分析物的相关系数均>0.99。MTF的定量限为0.009μg/mL，GPZ为0.009μg/mL，GLM为0.04μg/mL，PGZ为0.124μg/mL，RPG为0.044μg/mL。所开发的方法具有特异性、准确性，适用于所提及药物在其药品中的质量控制和常规分析。
