石油醚萃取结合pH沉淀法制备大黄游离蒽醌注射液

Preparation of free anthraquinones injection from rhubarb using methods of ligarine extraction and dopant sedimentation by pH

以大黄极细粉为原料,经酸化和超声波处理,回流提取制备大黄浸膏;采用石油醚萃取大黄游离蒽醌,调节pH值除去杂质得到纯品后制备大黄注射液;高效液相色谱检测大黄酸、大黄素、芦荟大黄素、大黄酚、大黄素甲醚的含量;氯化钠明胶法检测鞣质含量;同时根据药典(2005版)规定检查注射液的热源性、刺激性、LD50。结果表明注射液中大黄酸、大黄素甲醚、大黄素、芦荟大黄、大黄酚含量分别为0.223 6、1.788 2、0.834 2、0.491 3、5.401 3mg/mL;总蒽醌含量为8.738 6mg/mL;LD50为1.213 1g;鞣质含量低于0.05mg/L。动物试验表明该方法制备的注射剂符合注射要求。

The impalpable powder （75μm） of Rhubarb was handled with acid and supersonic wave, and extractum of rhubarb was prepared by recirculation extracting. Free anthraquinones was extracted with ligarine. Dopant was detached at pH value of 9 in water to prepare purified free anthraquinones injection. Concentrations of rhein, emodin, chrysophanol,physcion and aloe- emodin were determinated by high performance liquid chromatography （HPLC）. The pyrogenic characteristics, muscle irritation, LD50 of this injection were examined according to the ＂Pharmacopeia of China 2005 ＂. Tannin was detected with gelatin solution. Results were as follows ： concentrations of rhein, physcion, emodin, aloe - emodin,chrysophanol were 0.223 6, 1. 788 2, 0. 834 2, 0. 491 3, 5. 401 3mg/mL, respectively. Concentration of total anthraquinone was 8. 738 6mg/mL. LD50 was 1. 213 1g. Tannin content was lower than 0.05mg/mL. Animal experiments showed that the injection of rhubarb described above was satisfied with the demand of Pharmacopeia. It was showed that the method of combinative usage of ligarine extraction and dopant sedimentation by pH adjustment to prepare rhubarb injection was practicable.