HPLC-CAD法测定伐地那非原料药的含量及有关物质

Determination of the Content and Related Substances of Vardenafil by HPLC-CAD

目的:建立HPLC-CAD法测定伐地那非原料药的含量及有关物质。方法:采用Agilent ZORBAX Eclipse XDB C18色谱柱(250 mm×4. 6 mm,5μm),流动相:0. 01 mol·L^(-1)乙酸铵(乙酸调p H至6. 0)-乙腈,流速:1. 0 ml·min^(-1),柱温:35℃,CAD雾化器温度:35℃,进样量:20μl。结果:伐地那非主成分与各有关物质均能有效地分离,伐地那非的进样量在0. 408～10. 200μg内与峰面积呈良好的线性关系(r=0. 999 4),平均回收率为99. 2%(RSD=1. 5%,n=9);单个杂质限量定为0. 1%,杂质总量为0. 5%。结论:本法准确,简便,灵敏度高,可用于伐地那非原料药的含量测定以及有关物质检测。

Objective: To establish an HPLC-CAD method for the determination of vardenafil and its related substances. Methods:An Agilent ZORBAX Eclipse XDB C18 column(250 mm × 4. 60 mm,5 μm) was used,the mobile phase consisted of 0. 02 mol·L-1 ammonium acetate solution( adjusting p H to 6. 0 with acetic acid)-acetonitrile,the flow rate was 1. 0 ml·min-1,the column temperature was 35℃,the nebulization temperature of detector was 35 ℃,and the injection volume was 20 μl. Results: Vardenafil and all the related compounds could be well separated. The linear range of vardenafil was 0. 408-10. 200 μg( r = 0. 999 4),and the average recovery was 99. 2%( RSD = 1. 5%,n = 9). The single impurity limit was set at 0. 1% and the limit of total impurities was set at0. 5%. Conclusion: The method is accurate,convenient and sensitive,and can be applied in the determination of the content and related substances of vardenafil.