帕瑞昔布钠主要降解杂质-伐地昔布的HPLC测定方法研究

Study on the determinationthe major degradation impurities-valdecoxib in parecoxib sodium by HPLC method

目的建立高效液相色谱法测定帕瑞昔布钠的主要降解杂质及工艺杂质。方法采用Phenomenex C18(150 mm×4.6 mm,5μm)色谱柱,以乙腈-0.01 mol/L磷酸氢二钠溶液(pH=3.0)(40∶60,V/V)为流动相,检测波长为215 nm,流速1.0 ml/min。结果帕瑞昔布钠及其主要降解杂质伐地昔布在0.5μg/ml^5.0μg/ml范围内,浓度与响应值峰面积的线性关系良好,相关系数分别为r=0.9997和r=0.9992。平均加标回收率为100.2%±3.3%(n=9)。结论本方法准确度、精密度、灵敏度等均较好,可用于帕瑞昔布钠主要降解杂质的测定,能有效控制帕瑞昔布的质量。

Objective A RP- HPLC method was established for the determination of the major degradation impurities and process impurities in Parecoxib sodium. Methods The separation was performed on a Phenomenex C18column（ 150 mm ×4. 6 mm,5 μm）. The mobile phase was acetonitrile- disodium hydrogen phosphate buffer solution（ 0. 01 mol /L）（ pH3. 0）（ 40∶60,V/V）. The detection was carried out with a uv detector at 215 nm. The flow rate was 1.0 ml/min. Results The linear relationship between its major degradation impurities valdecoxib with the concentration of 0. 5 μg /ml - 5. 0 μg /ml and the response values of peak area was good,and the correlation coefficients were r = 0. 9997 and r = 0. 9992,respectively. The average recovery was 100. 2% ± 3. 3%（ n = 9）. Conclusion The method was proved to be accurate,sensitive and reliable,which can be used for determination of the major degradation impurities- valdecoxib in Parecoxib sodium. The method is used to effectively control the quality of parecoxib.