HPLC法测定利格列汀的S-异构体

Determination of S-isomer in Linagliptin by HPLC

目的:建立高效液相色谱法测定利格列汀原料药中S-异构体的方法。方法:采用AD-H色谱柱(250mm×4.6mm,5μm),流动相为乙醇-乙醇胺(100:0.1),柱温为35℃,流速为0.4mL·min^(-1),检测波长为220nm。结果:利格列汀S-异构体在0.0899~0.6744μg·mL^(-1)范围内与峰面积呈良好的线性关系(r=0.9996),低、中、高浓度平均回收率分别为101.8%、98.4%、96.0%,RSD分别为1.68%、1.63%、1.40%(n=3),检出限为0.18ng,日内、日间精密度RSD分别为3.4%和4.6%(n=6)。结论:该方法灵敏、准确,专属性强,可作为利格列汀原料药中的S-异构体含量测定方法。

To determine S - isomer in linagliptin by HPLC. Methods ：The chromatography separation was performed on a CHIRALPAK AD - H column （250mm×4.6mm, 5 μm） at 35℃, The flow rate was at 0.4 mL · min - 1, The mobile phase was ethanol - ethanolamine -- 100：0.1. The detection wavelength was 220nm. Results： S - isomer showed a good linearity at 0. 0899 - 0.6744μg·mL^-1. The average recovery of low, medium, high concentration of S - isomer was 101.8% ,98.4% and 96： 0% , RSD was 1.68%, 1.63% andl. 40% （ n = 3 ）, respectively. The limit for determination was 0.18ng and the RSD of intra - day and inter - day was 3.4% and 4.6% （ n = 6）, respectively. Conclusion： The method is simple and accurate for the determination of S -isomer in linagliptin.