梯度洗脱HPLC测定辛伐他汀片的含量和有关物质

目的建立辛伐他汀片含量测定及有关物质的检查方法。方法采用反相高效液相色谱法,色谱柱:SUPELCO C18柱(4.6mm×33mm,3μm),以乙腈-0.1%磷酸(50:50)为流动相A,0.1%磷酸乙腈溶液为流动相B,线性梯度洗脱,流速:3.0mL.min-1,检测波长238nm。结果辛伐他汀与洛伐他汀及强制破坏产生的降解产物均分离良好,辛伐他汀浓度在21.88～196.9μg.mL-1内,与峰面积呈良好的线性关系,回归方程A=65929ρ+4676,r=0.9996(n=7);日内精密度为0.54%(n=5);日间精密度为0.85%(n=5);平均回收率为99.55%(RSD=0.67%,n=9);样品溶液至少在3h内稳定;最低检测限为25.14ng.mL-1。结论该法专属性强,准确、灵敏,可用于辛伐他汀片的含量测定和有关物质检查。

Determination of Content and the Related Substances of Simvastatin Tablets by HPLC

OBJECTIVE To establish a method for determining the content and related substances of simvastatin tablets. METHODS The separation was carried out on a SUPELCO C₁₈ column (3 μm，4.6 mm×33 mm) with gradient elution. The mobile phase consisted of acetonitrile-0.1% phosphoric acid solution (50∶50) as the mobile phase A, and 0.1% phosphoric acid in acetonitrile as the mobile phase B. The flow rate was at 3.0 mL·min-1and the detection wavelength was at 238 nm. RESULTS The resolution between the peak of losvatatin and simvastatin was above 5.0. The linear range of the method was 21.88-196.9 μg·mL-1 and the regression equation was A=65 929ρ+4 676 (r=0.999 6， n=7).The average recovery was 99.55%（RSD=0.67%, n=9） and the limit of detection was 25.14 ng·mL-1. The sample solution was stable within 3 h. CONCLUSION The method is specific, accurate, sensitive and can be used for the determination of content and related substances of simvastatin tablets.