梯度洗脱HPLC测定辛伐他汀片的含量和有关物质  

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

作　　者：郑金琪[1] 郑国钢[1] 李会林[1] 黄豆[2] 胡楚楚[1] 

机构地区：[1]浙江省食品药品检验所,杭州310004 [2]浙江大学城市学院医学与生命科学学院,杭州310015

出　　处：《中国药学杂志》2010年第9期702-705,共4页Chinese Pharmaceutical Journal

摘　　要：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。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^-1nd 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.

关 键 词：辛伐他汀片 含量测定 有关物质 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]