替硝唑原料的精制及纯度分析  

Purification of tinidazole and its analysis by HPLC

作　　者：邹莹[1] 刘永琼[1] 祝宏[1] 王剑[1] 

机构地区：[1]武汉工程大学化工与制药学院湖北省新型反应器与绿色化学工艺重点实验室,湖北武汉430074

出　　处：《中国医院药学杂志》2007年第9期1233-1235,共3页Chinese Journal of Hospital Pharmacy

摘　　要：目的:研究提高替硝唑原料药纯度至99.9%以上的精制方法及相关纯度分析方法。方法:利用替硝唑在不同溶剂中溶解度的差异,研究用重结晶法来提高替硝唑原料纯度的方法,并用HPLC主成分自身对照法监测精制后的替硝唑纯度:供试品溶液(1g.L-1)的色谱图中如显示杂质峰,各杂质峰峰面积的和不大于对照溶液(1μg.mL-1)的主峰面积,即精制品的纯度达到99.9%以上。结果:确定了精制方法的最佳工艺流程及条件,使替硝唑注射液用药的纯度(不得少于99.0%)提高到99.9%以上,精制平均收率为88.81%。结论:该方法成熟可行,提高替硝唑原料纯度99.9%以上。OBJECTIVE To develop a method to purify tinidazole（not less than 99. 0 % ）and use self-calibration method with HPLC to monitor the purity of refined tinidazole. METHODS A re-crystallization method to improve the purity of tinidazole was presented, the method based on the difference of its solubility in different solvents. The average purification yield was 88. 81%. The self-calibration method with HPLC was used to monitor the purity of refined tinidazole., the total areas of all impuity peaks in the chromatogram obtained with test solution（1 mg. mL^-1 ） were no more than the area of the principal peak in the chromatogram obtained with reference solution（1 μg· mL^- 1 ）, then the aim was reached. RESULTS An optimum technological flowsheet and conditions were developed above. The average purification yield is 88. 81%. CONCLUSION A mature and feasible method is developed to improve the purity of tinidazole and the results of HPLC proved that our aim was reached.

关 键 词：替硝唑 纯化 高效液相色谱法 自身对照法 

分 类 号：R978.61[医药卫生—药品] R927.11[医药卫生—药学]