格列美脲盐酸二甲双胍复方片中格列美脲有关物质研究

Study on related substance of glimepiride in glimepiride/metformin hydrochloride combination tablet

目的:建立HPLC法测定格列美脲盐酸二甲双胍复方片中格列美脲有关物质,并对新增杂质X归属进行研究。方法:色谱柱:Agilent XDB C1(84.6 mm×250 mm,5μm);流动相:磷酸盐缓冲液为6.4 mmol/L磷酸二氢钠(pH=6.8)—乙腈梯度洗脱,柱温:35℃;流速:1.0 mL/min;检测波长:228 nm。应用HPLC-MS法对杂质X归属进行研究。结果:在选定的色谱条件下,格列美脲主峰与各杂质峰间分离良好;杂质X为格列美脲和盐酸二甲双胍原料相互作用的结果。结论:所建方法准确、灵敏、可靠,可用于格列美脲盐酸二甲双胍片复方片中格列美脲有关物质的检查。

Objective： To establish a HPLC method for the determination of glimepiride related substance in glimepiride/metformin hy- drochloride combination tablet and identify the impurity X. Methods： Agilent XDB Ct8 column （4.6 mm×250 mm, 5 μm）was used with acetonitrile-6.4 mmol/L phosphate buffer solution （pH 6.8 adjusted with ammonia solution） as mobile phase with gradient elution at a rate of 1.0 mL/min. The column temperature was 35 ℃ and the detection wavelength was 228 nm. The impurity X was identified by HPLC-MS. Results： Complete separation was achieved for the main components and related substance. Impurity X was the result of the interaction of glimepiride and mefformin hydrochloride raw materials. Conclusion： The method is accurate, sensitive and reliability ,which can be used for the quality control in glimepiride/mefformin hydrochloride combination tablet.