摘要
目的:提取斑蝥素,合成斑蝥素羧基衍生物,探究合成反应最佳条件及产率并比较二者的胃毒毒力的强弱。方法:有机溶剂萃取方法提取斑蝥素,在单因素不同的体系中与β-丙氨酸进行缩合反应,且用GC、TLC、UV、MS、NMR等对提取物及反应产物进行鉴定,并通过改良寇氏法测定二者的LD50以比较其毒性。结果:提取的斑蝥素纯度达98.53%,缩合产物为N-羧乙基斑蝥酰亚胺。最佳反应条件:n(斑蝥素)/n(β-丙氨酸)=1/1.2;媒介溶剂与催化剂均为Et3N,最佳用量为1mol的斑蝥素需72mL的Et3N,125～150℃下脱水反应4～5h,产率可达74.40%。衍生物对小鼠的胃毒力仅为斑蝥素毒性的1/400。结论:可以利用药用斑蝥虫体提取高纯度斑蝥素,并用以合成低毒性的斑蝥素羧基衍生物,且在最佳条件下有较高产率。
Objectives ：To extract the cantharidin and synthesize its carboxyl derivative, optimize the reaction condition and determine the derivative yield under this condition, and compare the stomach toxicity between cantharidin and its derivative. Methods： Extract the cantharidin by organic reagent, then, use it to condense with β - Ala in different systems with a single factor changed;identify the cantharidin and its derivative with GC, TLC, UV, MS and NMR;compare the toxicity by determining the two chemicals＇ LD50 in mice with modified Kaber method. Results： The purity of the extracted cantharidin reached 98.53% ntharidimide, the yield reached 74. 4% in the optimized , the product of the condensation was N - carboxyethylcacondition with the ratio of cantharidin to β - Ala was 1 ： 1.2 and with the Et3 N as intermediary agent and catalyzer that 1 mol cantharidin needed 72 mL Et3 N to catalyze in 125 - 150℃ for 4 -5 h;the stomach toxicity of the derivative was only 1/400 of that of cantharidin. Conclusions： It is feasible to extract the high purity cantharidin from polypide powder of cantharis. The synthesized carboxyl derivative showed with much lower toxicity, and, the yield can arrive as high as 74. 4% in optimized condition.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第1期25-30,共6页
Chinese Journal of Pharmaceutical Analysis
