丁香苦苷冻干粉针的处方优化及制备工艺的研究

目的:研究适合注射用丁香苦苷冻干粉针的处方配比和制备工艺。方法:以产品外观,复水性,含量等为指标,运用正交试验法优化其处方配比;采用真空冷冻干燥法制备其样品,用高效液相色谱法检测其含量,并对制备条件如装量、共晶点、预冻温度、升华温度、解吸温度等进行研究。结果:经优化,确定丁香苦苷含量为8%(A2),赋形剂用量为5%甘露醇(B2),装量为2.5mL(C3),西林瓶规格为7mL(D1);生产工艺为pH值为7.0,-45℃下预冻、-30℃下升华干燥和25℃时解吸干燥。结论:该工艺制备的丁香苦苷冻干粉针符合《中国药典》(2005版)冻干粉针的相关规定。

Optimization of Formulation and Freeze-drying Process of Clove Gentiopicroside for Injection

Objective： To study a suitable formulation and freeze-drying process of Clove gentiopicroside for injec- tion. Methods： The formulation was optimized according to the appearance, clarity and content of the production by us- ing orthogonal analysis. The vacuum freeze-drying method was modified by changing the process conditions such as liq- uid volume in bottle, the pre-ffeezing temperature, sublimating temperature and temperature of desorption. The content of the Clove gentiopicroside was detected by HPLC. Results： The formulation consists of Clove gentiopicroside 8% （A2） and mannitol 5%（B2）, and 2.5 mL（C3） liqud was filled in 7 mL bottle（D1）. The acceptable freeze-drying process is that liquid pH value was 7.0, pre-freezing temperature was -45 ℃,sublimating temperature was -30 ℃, and desorption temperature was 25 ℃. Conelusion： The lyophilized agent prepared based on this formulation and this process meets the requirements of the Chinese Pharmacopoeia 2005.