石蒜生物碱的双向薄层色谱分析及气质联用鉴定

摘要

建立双向薄层色谱分离石蒜多种生物碱组分的方法,并初步制备了生物碱单品.研究了石蒜生物碱各组分分离的单向及双向展开剂,结果表明:单向薄层色谱分离以氯仿∶甲醇∶氨水=9∶1∶0.2的展开剂分离效果最好,分离出的斑点数为13个.双向薄层色谱分离以乙酸乙酯∶甲醇∶氨水=9∶1∶0.2为第1向展开剂,氯仿∶甲醇∶氨水=9∶1∶0.2为第2向展开剂,分离石蒜生物碱效果最好,斑点数多达16个,且非常清晰.利用该方法对石蒜不同器官中生物碱进行了分析,结果显示:根中生物碱种类最多且含量最高,鳞茎其次,叶最低.经HPLC对分离得到的16个斑点进行检测,其中15个生物碱色谱峰明显,8种生物碱的纯度在90％以上,其中5种的纯度达93％以上,经气质联用鉴定,分别是石蒜碱、力克拉敏、加兰他敏、多花水仙碱和普鲁维因.此法适于石蒜生物碱组分的分析及微量制备.%A method for the identification and preliminary preparation of L.radiata alkaloids was established.The one-dimensional and two-dimensional thin-layer chromatography (TLC) analysis were used to separate the alkaloids of L.radiata.The results showed that the optimized eluent was CHCI3/MeOH/NH3·H2O (9 ∶ 1 ∶ 0.2,V/V/V) for onedimensional TLC.The optimized eluent was EtOAc/MeOH/NH3·H2O (9∶1∶0.2,V/V/V) in first direction and CHCl3/MeOH/NH3·H2O (9∶1∶0.2,V/V/V) in the second direction for two-dimensional TLC.The two-dimensional TLC exhibited a better seperation effect than the one-dimensional TLC.Applied the two-dimensional TLC,16 spots were seperated.The method was used to analyze the alkaloids in different parts of L.radiata,which showed that alkaloids types and amounts were the highest in roots,followed by bulbs,and finally leaves.Applied the method,the seperated 16 spots were detected by HPLC.The result showed that 15 alkaloids chromatographic peaks were obvious and the purities of 8 kinds were above 90％,of which the purities above 93％ detected by GC-MS were lycorine,lycoramine,galanthamine,tazettine,pluviine.The method was suitable for analyzing and preparing L.radiata alkaloids.