GC法测定帕瑞昔布钠原料药中8种残留溶剂

GC determination of 8 kinds of residual solvents in parecoxib sodium active pharmaceutical ingredient

目的测定帕瑞昔布钠原料药中正己烷、甲基叔丁基醚、三乙胺、四氢呋喃、乙酸乙酯、二氯甲烷、乙醇和乙基苯共8种残留溶剂含量。方法采用毛细管气相色谱法,检测器为氢火焰离子化检测器,以氮气为载气进行程序升温,用外标法计算帕瑞昔布钠原料药中的8种残留溶剂。结果在15 min内,8种残留溶剂色谱峰得到有效分离,在一定质量浓度内,8种残留溶剂的线性关系均良好(r>0.999),日内(n=6)和日间精密度(n=12)的RSD均小于5%,加样回收率结果(n=9)在80%~120%内,RSD值均小于5%,不同批次原料药残留溶剂检查结果均符合要求。结论该方法为帕瑞昔布钠原料药残留溶剂检查质量标准的制定提供了依据,通过该方法检查的帕瑞昔布钠原料药可用于注射用帕瑞昔布钠的生产。

Objective To determine the residual solvents in parecoxib sodium active Pharmaceutical Ingredient,the residual solvents including Hexane,methyl tert butyl ether,three ethylamine,tetrahydrofuran,ethyl acetate,dichloromethane,ethanol and ethyl benzene. Methods In this experiment,the capillary gas chromatography was adopted,the hydrogen flame ionization detector was used,and the nitrogen was used as carrier gas of the programmed Temperature gas chromatography method,8 kinds of residual solvents of parecoxib sodium rawmedicine had been calculated according to the external standard method. Results In15 min,8 kinds of residual solvent peak were effectively separated,within a certain concentration range,the linear relationship of the 8 kinds of residual solvents were good（ r 0. 999）,the Intraday precision RSD（ n = 6） and day to day precision RSD（ n = 12） were less than 5%,The recovery of sample addition（ n =9） was between 80%-120%,RSD values were less than 5%,The results of different batches of rawmaterial residual solvents were in accordance with the requirements. Conclusion This method can provide basis for the establishment of the parecoxib sodium API quality standard,parecoxib sodium API examined by this method can be used for the production of Parecoxib Sodium for Injection.