HPLC法测定维格列汀原料药中的有关物质

Determination of related substances in vildagliptin by HPLC

目的:建立维格列汀原料药有关物质的HPLC测定方法。方法:采用Agilent Eclipse Plus C18色谱柱(4.6 mm×250 mm,5μm)对降解杂质和工艺杂质进行定量分析,以10 mmol·L^(-1)辛烷磺酸钠(加入0.1%磷酸调pH至2.1)-乙腈为流动相,梯度洗脱,流速1.0 m L·min^(-1),检测波长为210 nm。结果:主峰与各杂质峰间能达到基线分离,维格列汀质量浓度在1.521 0~20.280μg·m L^(-1)范围内与峰面积呈良好的线性关系(r=0.999 8),最低检测限为0.5μg·m L^(-1);3批样品有关物质测定结果显示,已知杂质含量均低于0.1%。结论:方法学验证结果表明,本法可作为维格列汀质量控制的方法。

Objective：To establish an HPLC method for determination of the related substances in vildagliptin.Methods：The test for degradation and process impurities was based on an Agilent Eclipse Plus C18（4.6 mm×250 mm,5 μm）column;the mobile phase consisted of 10 mmol·L-（-1） sodium octanesulfonate solution（adjusted to pH 2.1 with 0.1% phosphoric acid）-acetonitrile with gradient elution at the flow rate of 1.0 m L·min-（-1）;the detection wavelength was 210 nm.Results：Chief peak and every impurity peak were separated well.A good linearity was observed over the range of 1.521 0-20.280 μg·m L-（-1）（r=0.999 8）,the LOD was 0.5 μg·m L-（-1）;The determination results of the three batch of samples showed that the impurity were less than 0.1%.Conclusion：Methodology validation results proved that the established determination method can be used for quality control of vildagliptin.