HPLC法同时测定琥珀酸曲格列汀中9个杂质的含量

Simultaneous Determination of Nine Impurities in Tragaliptin Succinate by HPLC

目的:建立高效液相色谱法同时测定琥珀酸曲格列汀中9个杂质的含量。方法:采用Welch Utimate AQ C18(4.6 mm×250 mm,5μm)色谱柱,以0.1%磷酸溶液-乙腈为流动相,梯度洗脱,流速1.0 mL·min^(-1),柱温35℃,检测波长230 nm。结果:该药与已知杂质Ⅰ~Ⅸ色谱峰之间的分离度良好;该药和已知杂质Ⅰ~Ⅸ分别在各自的线性范围内线性关系均良好(r^(2)≥0.9999),杂质Ⅰ~Ⅸ的校正因子分别为1.3、0.9、0.5、1.2、1.2、1.0、2.1、2.3、1.0,且该药和已知杂质Ⅰ~Ⅸ的平均回收率均在99.0%~101.0%。结论:该方法专属性强,重复性好,可用于测定该药中的有关物质。

Objective:To establish an HPLC method for simultaneous determination of 9 impurities in tragaliptin succinate.Methods:The analysis was performed by HPLC with a Welch Utimate AQ C18 column(4.6 mm×250 mm,5μm),the mobile phase was an acetonitrile-0.1%phosphoric acid aqueous solution gradiently eluted at 1.0 mL·min^(-1),the column temperature was 35℃and the detection wavelength was 230 nm.Results:The resolutions between the peaks of tragaliptin succinate and nine known impuritiesⅠ-Ⅸwere good.Tragaliptin succinate and the known impuritiesⅠ-Ⅸhad good linear relationships in their respective linear ranges(r2≥0.999)with average recoveries at 99.0%-101.0%,the correction factors for the impuritiesⅠ-Ⅸwere 1.3,0.9,0.5,1.2,1.2,1.0,2.1,2.3 and 1.0.Conclusion:This method is specific and accurate,and can be used to detect related substances in tragaliptin succinate.