维格列汀有关物质检查

Study on Determination of the Related Substances in Vildagliptin

建立了测定维格列汀有关物质检查方法。用十八烷基硅烷键合硅胶为填充剂,以磷酸盐缓冲液(取磷酸氢二铵2.64 g,溶于1000 m L水中,用稀氨水或磷酸溶液调节p H值至8.0±0.05)-甲醇(90∶10)为流动相A,甲醇为流动相B;进行梯度洗脱。流速1.0 m L·min-1,柱温40℃,检测波长210 nm。对维格列汀3种杂质进行定量检查。结果表明:各杂质与主成分能完全分离,杂质Ⅰ、Ⅱ、Ⅲ检测限分别为1.1、1.2、1.2 ng(S/N=3),回收率分别为96.8%、103.6%、107.1%,浓度与峰面积均呈线性(r>0.999)。结论本法准确、简便、快速,可用于维格列汀有关物质检查。

A method for determination of the related substances in Vildagliptin was established. It was determined on HPLC. The C18 was used as analytical column. Phosphate buffer （containing 2.46 g of diammonium hydrogen phosphate in 1 litre of water, adjusted to pH 8.0±0. 05 with ammonium hydroxide solution or phosphoric acid） and methanol （90 ： 10） were used as mobile phases A, methanol were used as mobile phases B, with gradient elution. The column temperature was kept at 40 ℃. The flow rate was 1.0 mL · min^-1. The detection wavelength was set at 210 nm. Results showed that Vildagliptin and its impurities could be separated with all related substances completely. The limits of detection was 1.1, 1.2, 1.2 ng （ S/N = 3 ） for impurity Ⅰ , Ⅱ , Ⅲ. Their linearities were good, with their recoveries 96.8%, 103.6%, 107.1%, respectively. The method is accurate and sensitive, and can be used for the related substances in Vildagliptin.