高效液相色谱法同时测定奥湿克片中两组分的含量及有关物质

RP-HPLC simultaneouly determination of diclofenac sodium,misoprostol and its related impurities in compound misoprostol tablet

目的 :测定奥湿克片中米索前列醇和双氯芬酸钠的含量及有关物质。方法 :采用RP HPLC ,用岛津Shim PackCLC C8柱 (4.6mm× 1 5mm ,5 μm) ;流动相 :乙腈 甲醇 pH 3.0缓冲液 (2 2∶36∶42 ) ,检测波长 :2 0 0nm ,有关物质B型米索前列醇 (SC 331 88) 2 80nm。结果 :米索前列醇和双氯芬酸钠分别在 1 0 .2～ 1 6 3.2 μg·ml-1(r =0 .9995 ,n =9)和 1 .2 9～ 2 0 .6 μg·ml-1(r =0 .9997,n =9)浓度范围内呈线性关系。米索前列醇和双氯芬酸钠的平均回收率 (n =6 )分别为 1 0 0 .0 % ,1 0 0 .6 % ;RSD分别为 0 .6 % ,0 .7% ,同时测定米索前列醇的有关物质。结论 :方法简便、准确。

OBJECTIVE:To develop an assay for the determination of diclofenac sodium,misoprostol and misoprostol related impurities in compound misoprostol tablet.METHODS:A RP HPLC was used on Shim Pack CLC C 8 column with a mobile phase of acetonitrile methanol pH 3.0 triethylamine buffer(22∶36∶42) and the detection wavelength at 200 nm(SC 33188 at 280 nm).RESULTS:The standard curves for misoprostol and diclofenac sodium were linear over the range of 10.2～163.2 μg·ml -1 ( r =0.9995, n =9);1.29～20.6 μg·ml -1 ( r =0.9997, n =9),respectively.The average recoveries of misoprostol and diclofenac sodium were 100.0%,100.6%;with RSD 0.6%,0.7%,respectively.Diclofenac sodium,misoprostol and its related impurities could be determined simultaneously.CONCLUSION:The method is convenient,accurate and precise.