Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, Beni-Suef, Egypt.
Chemistry Department, Faculty for Girls, Ain Shams University, Cairo, Egypt.
J Sep Sci. 2021 Feb;44(4):833-842. doi: 10.1002/jssc.202000937. Epub 2021 Feb 2.
Two simple, sensitive, and reproducible methods were developed for the determination of alogliptin and metformin hydrochloride in presence of metformin impurity "melamin" in pure form and in pharmaceutical formulation. Method (A) was a thin layer chromatographic method in which separation was achieved using ethyl acetate-methanol-formic acid (6:3.8:0.2, by volume) as a developing system followed by densitometric scanning at 230 nm. Method (B) was a high-performance liquid chromatography method; separation was achieved on C column, the mobile phase consisted of a mixture of sodium lauryl sulfate buffer 0.1% w/v, pH 3: methanol in the ratio 70:30, v/v and measurement was done at 220 nm. System suitability testing parameters were calculated to ascertain the quality performance of the developed chromatographic methods. The proposed methods have been validated regarding accuracy, precision, and selectivity, moreover they have been successfully applied to Westirizide tablets containing both alogliptin and metformin hydrochloride, results indicate that there was no interference from additives. No significance difference was found when these methods were compared to the reported one.
两种简单、灵敏且重现性良好的方法被开发出来，用于在纯品和药物制剂中测定阿格列汀和盐酸二甲双胍，同时存在二甲双胍杂质“三聚氰胺”。方法（A）为薄层色谱法，采用乙酸乙酯-甲醇-甲酸（6:3.8:0.2，体积比）作为展开系统，在 230nm 处进行密度扫描。方法（B）为高效液相色谱法，采用 C 柱进行分离，流动相由 0.1% w/v 十二烷基硫酸钠缓冲液 pH 3：甲醇（70:30，v/v）组成，在 220nm 处进行检测。系统适用性测试参数的计算旨在确定所开发的色谱方法的质量性能。对所提出的方法进行了准确性、精密度和选择性验证，此外，还成功地应用于含有阿格列汀和盐酸二甲双胍的 Westirizide 片剂，结果表明添加剂没有干扰。与已报道的方法相比，这些方法没有发现显著性差异。
