UPLC法测定卡格列净原料药的有关物质

Determination of Related Substances in Canagliflozin by UPLC

目的:建立一种超高效液相色谱法(UPLC),用于测定卡格列净原料药中的有关物质。方法:采用Waters Acquity BEH C18(3.0 mm×150 mm,1.7μm)色谱柱,以0.1%磷酸溶液为流动相A,乙腈-甲醇(体积比80︰20)为流动相B;采用梯度洗脱方式进行洗脱;流速为0.4 mL/min;检测波长为225 nm;柱温为30℃。结果:卡格列净及其已知杂质(KGL-A、KGL-C、KGL-D、KGL-G)在定量限~0.90μg/mL浓度范围内呈良好的线性关系;KGL-A、KGL-C、KGL-D、KGL-G的平均回收率为91.1%~103.0%。结论:该方法专属性强、灵敏度高、重现性好、操作简便、分析速度快,检测结果准确可靠,适用于测定卡格列净原料药的有关物质。

Objective:To establish an Ultra Performance Liquid Chromatography(UPLC)method for determination of Canagliflozin API related substances.Methods:The analysis was performed on a Waters Acquity BEH C18(3.0 mm×150 mm,1.7μm).The mobile phase A was 0.1 percent solution of phosphoric acid,the mobile phase B was Acetonitrile and Methanol(80∶20).Gradient elution method was used for elution.The flow rate of mobile phase was 0.4 mL/min,the detection wavelength was 225 nm and the column temperature was 30℃,respectively.Results:The chromatographic peak area and concentration of Canagliflozin API、KGL-A、KGL-C、KGL-D、KGL-G showed a good linear relationship at the range of LOQ~0.90μg/mL.The average recovery of KGL-A、KGL-C、KGL-D、KGL-G were 91.1%~103.0%.Conclusion:The method is specific,sensitive,good reproducibility,simple operation,high analysis speed,accurate and reliable detection results.It is suitable for determination of related substances of Canagliflozin API.