HPLC法测定依普利酮片含量及有关物质  

HPLC determination of eplerenone tablets and its related substances

作　　者：杜明荦[1] 连莹[1] 

机构地区：[1]河南省食品药品检验所,郑州450003

出　　处：《医药论坛杂志》2017年第7期21-23,共3页Journal of Medical Forum

摘　　要：目的建立依普利酮片有关物质和含量测定的HPLC测定方法。方法采用Sepax GP-C18(4.6mm×250 mm,5μm)色谱柱,以10mmol/l醋酸铵为流动相A,乙腈-甲醇(1∶1)为流动相B,241nm波长检测,线性梯度洗脱进行有关物质检查,等度洗脱进行含量测定,LC-MS/MS法鉴定有关物质。结果依普利酮的线性范围为2~250μg/ml(r=1.000),平均回收率为99.9%,RSD为0.9%,检测限为0.05μg/ml,精密度与24h稳定性RSD均小于2%;依普利酮与强制降解产物分离度良好。结论本方法简便、灵敏、重复性好,结果准确可靠。可作为依普利酮片含量测定和有关物质的检查方法,其主要降解杂质为水解物。Objective To establish an HPLC method for the determination of eplerenone tablets and its related substances. Methods The analysis was performed on a Sepax GP-C18 column（4. 6mm × 250 mm,5μm） with the mobile phase consisted of solvents A（10mmol/l ammonium acetate） and solvent B（ methanol∶ acetonitrile = 1∶1） at the detection wavelength of 241 nm. The related substances was determined by gradient elution while content determination by isocratic elution. The major related substances were identified by LC-MS/MS. Results The linear range for eplerenone was 2 ~ 250μg/ml（ r = 1. 000）. The average recovery was 99. 9%（ RSD = 0. 9%,n = 9）,the LOD was 0. 05μg/ml,and the RSD of precision and 24 h stability were both below 2%. Satisfactory resolutions between eplerenone and its forced degradation products were achieved. Conclusion This method is simple,sensitive,reproducible,and the results are accurate and reliable. It can be used for the determination of eplerenone tablets and its related substance. The major degradation product was hydrolysate of eplerenone.

关 键 词：依普利酮 有关物质 含量测定 高效液相色谱 

分 类 号：R927.2[医药卫生—药学]