高效液相色谱法测定维格列汀R型异构体的含量

Determination of vildagliptin R-isomer by HPLC

目的:建立维格列汀R型异构体含量的高效液相色谱检测方法。方法:采用高效液相色谱(HPLC)法测定,色谱柱为ChiralpakIC(250mm×4.6mm,5μm);流动相为乙醇-正己烷-叔丁基胺(90∶10∶0.1);流速为0.7ml/min;柱温为25℃;检测波长210nm。结果:维格列汀与其R型异构体峰分离良好,异构体在0.4~2.4μg/ml浓度范围内,浓度与峰面积呈良好的线性关系,异构体的定量限为4.0ng,检测限为1.3ng。结论:该方法简便易行,灵敏度高,可用于维格列汀R型异构体含量的检测。

Objective: In this paper, we established a high performance liquid chromatograph method for determining of the R- enantiomer content of vildagliptin. Methods: The high performance liquid chromatography was used. The determination was performed on Chiralpak IC(250 mm×4.6 mm,5 μm)column, and the mobile phase was composed of solution of ethanol : n-hexane: tert-butylamine (90∶10∶0.1). The flow rate was 0.7 ml/min, the column temperature was 25 ℃ and the detection wavelength of 210 nm. Results: The peaks of vildagliptin and its R- isomer were well separated. Within the range of 0.4~2.4 μg/ml, the concentration of the R- isomer showed a good linear relationship between the concentration and the peak area. The limit of quantification was 4.0 ng, and the limit of detection was 1.3 ng. Conclusion: The established method was simple, feasible and highly sensitive. It can be used for determining the R- enantiomer content of vildagliptin.