论文部分内容阅读
称取金龟子绿僵菌干燥菌丝体200 g,甲醇浸泡24 h,减压浓缩至浸膏,c(HCl)=1 mol/L盐酸溶解后依次用环己烷、氯仿和正丁醇分段萃取,酸水液上732型强酸性阳离子交换树脂柱,c(NH3.H2O)=1 mol/L氨水洗脱并挥干,得到总生物碱。总生物碱用无水乙醇索氏提取24 h,挥干后干燥物上硅胶柱,V(氯仿)∶V(甲醇)∶V(氨水)∶V(水)=70∶26∶2∶2混合溶剂洗脱,薄层色谱检测发现101～142份洗脱液含有苦马豆素,合并101～142份洗脱液并挥干,氨性氯仿反复溶解,冷冻干燥后在110℃、-0.094 Pa真空条件下升华,得到白色针状结晶3.6mg。经薄层色谱检测、熔点测定及气相色谱检测,可确定该白色针状结晶为苦马豆素,苦马豆素的提取率为18μg/g。气相色谱法测定金龟子绿僵菌干燥菌丝体中苦马豆素的质量分数为0.212%。
Weigh 200 g dried mycelium of M. anisopliae, immersed in methanol for 24 h, concentrated under reduced pressure to extract, dissolved in hydrochloric acid (c) = 1 mol/L, followed by sequential extraction with cyclohexane, chloroform and n-butanol. The acidic aqueous solution was columned on a 732-type strongly acidic cation exchange resin column and eluted with c(NH3.H2O)=1 mol/L aqueous ammonia and evaporated to give total alkaloids. The total alkaloids were extracted with ethanol soxhlet for 24 h, evaporated to dryness and then dried on a silica gel column. V (chloroform): V (methanol): V (ammonia): V (water) = 70:26:2:2 Solvent elution, thin layer chromatography revealed 101 to 142 eluates containing swainsonine, combined with 101 to 142 eluates and evaporated to dryness, the ammoniacal chloroform was repeatedly dissolved and lyophilized at 110°C, -0.094 Pa. Sublimation under vacuum gave 3.6 mg of white needles. By thin layer chromatography, melting point determination and gas chromatography, the white needle crystals were identified as swainsonine, and the extraction rate of swainsonine was 18 μg/g. The mass fraction of swainsonine in dried mycelia of Metarhizium anisopliae was 0.212% by gas chromatography.