一种传统复方中药冻干粉的研制.pdf

摘 要
为了将一种传统复方中药制备成冻干粉粉针剂，并对其进行质量研究及稳定性考
察。本试验首先采用水醇法对中药提取液进行除杂；并采用正交试验方法，以药液中主
要成分（绿原酸、表告依春及苦参碱）的转移率及鞣质的去除情况为指标，对明胶法除
鞣质中的药液浓缩比例、pH 值和反应温度三个因素进行考察；采用单因素试验，对保护
剂的种类和用量，药品冻干浓度、药液的 pH 值进行筛选，确定冻干配方；通过冻干机
测定隔板温度和样品温度，绘制降温曲线确定样品的共熔点；采用正交试验方法，以冻
干率为考察指标确定最佳冻干工艺参数；应用高效液相色谱法定量分析冻干粉中绿原酸、
表告依春及苦参碱的含量来考察冻干粉的质量；通过溶血性试验、过敏性试验、刺激性
试验考察冻干粉的安全性；通过影响因素试验、加速试验及长期试验对冻干粉的稳定性
进行考察。
试验结果：水醇法不能将药液中的鞣质完全去除，在药液浓缩比例为 1:3、药液 pH
值为 7、反应温度为 80℃时，药液中有效物质的转移率较高，明胶法去除鞣质效果良好；
冻干配方为：冻干药液浓度 20%，最佳保护剂为 10%甘露醇，最佳 pH 值为 6～7；样品
的最低共熔点为：-3℃～-8℃；最佳冻干工艺为：-50℃预冻 5 h、-20℃低温升华干燥 14
h，30℃解析干燥 10h；在此工艺条件下获得的冻干粉成型性、外观、复水性均良好，主
成分含量均一稳定，无溶血、过敏及刺激性反应；该冻干粉在高温试验、光照试验、加
速试验以及长期试验中稳定性均良好。
综上所述，该冻干粉配方合理，制备工艺可行，质量安全可控，稳定性良好。
关键词：复方中药；冻干粉；安全性；稳定性








I
Abstract
The objective was to prepare a compound traditional Chinese medicine lyophilized
powder, and study the quality and stability of the lyophilized water alcohol
precipitation was applied to traditional Chinese medicine extract. Orthogonal test method was
used to the removal of tannin by gelatin method, taking transfer rate of the main component
(chlorogenic acid, table to spring and matrine) in the liquid and the removal of tannic acid as
index, concentrate proportion of Chinese medicine extract, pH and temperature was explored.
Using orthogonal experiment method,freeze-drying process parameters can be calculated by
freeze-dried rate;High performance liquid chromatography (HPLC) was applied to content
analysis of chlorogenic acid,epigoitrin and evaluate the security by testing
the vessel stimulation, hypersensitivity and hemolytic test in stability was evaluated
by classical stress test, accelerated test and and long-term test.
Test results: tannide can not be completely removed by wat