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

作　　者：徐在品[1] 彭广能[2] 郑静[2] 邓小燕[3] 杨小生 罗鹏[1] 高俊波[1] 赵伟[1] 周皓[2] 

机构地区：[1]贵州大学动物科学学院,贵州贵阳550025 [2]四川农业大学动物医学学院,四川雅安625014 [3]北京航空航天大学生物工程系,北京100083 [4]中国科学院天然产物化学重点实验室,贵州贵阳550002

出　　处：《山地农业生物学报》2008年第4期340-344,共5页Journal of Mountain Agriculture and Biology

基　　金：国家自然科学基金项目资助(10572029;10772054);国家自然科学基金重点项目资助(10632010)

摘　　要：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.

关 键 词：大黄注射液 大黄游离蒽醌 总蒽醌 鞣质 HPLC 

分 类 号：Q949.744.06[生物学—植物学] R284.2[医药卫生—中药学]