【摘要】 应用高速逆流色谱分离制备大麻药的化学成分,以石油醚∶乙酸乙酯∶乙醇∶水(1∶1.2∶1.2∶1,V/V)为两相溶剂系统,上相为固定相,下相为流动相,流速2.0 mL/min,主机转速800 r/min,分离温度30℃,检测波长280 nm。以此分离条件经一步洗脱从400 mg大麻药粗提物中制备得到95.3 mg和84.5 mg的两个单体化合物,经理化反应和光谱分析分别鉴定为(2S)-5,2′,6′-三羟基-8-异戊烯基-6,7-(3-异戊烯基-2,2-二甲基-1-酮-环己二烯)-二氢黄酮(1)和(2S)-5,2′,6′-三羟基-8-异戊烯基-6,7-(3-异戊烯基-2,2-二甲基吡喃)-3′,4′-(2,2-二甲基-1-酮-环己二烯)-二氢黄酮(2)。所得的化合物1和2均为新化合物。更多还原

【Abstract】 The separation and isolation of chemical constituents from Dolichos tenuicaulis(Baker) Craib by high-speed counter-current chromatography(HSCCC) were achioved.The solvent system composed of petroleum ether∶ethyl acetate∶ethanol∶water(1∶1.2∶1.2∶1,V/V) was selected to purify the compounds,the upper phase was used as the stationary phase,the lower phase was used as the mobile phase at a flow rate of 2.0 mL/min,and the apparatus was controlled at 800 r/min and 30℃,and the effluent was monitored at 280 nm.Under the optimized conditions,two pure compounds with the amounts of 95.3 mg and 84.5 mg were produced from 400 mg crude sample only in one run,and the chemical structures of the targets were elucidated as(2S)-5,2′,6′-trihydroxy-8-prenyl-6,7-(3-prenyl-2,2-dimethyl-1-keone-cyclohexadiene)-flavanone(1) and(2S)-5,2′,6′-trihydroxy-8-prenyl-6,7-(3-prenyl-2,2-dimethylpyrano)-3′,4′-(2,2-dime-thyl-1-keone-cyclohexadiene)-flavanone(2) by physico-chemical properties and spectra data.This separa-tion method was simple,and the compounds 1 and 2 were new compounds.更多还原