1-脱氧野尻霉素提取精制工艺的研究  

Study on the extraction and purification of DNJ from Morus alba L

作　　者：刘韦鋆[1] 赵骏[1] 高秀梅[1] 刘美平[1] 曾森[1] 

机构地区：[1]天津中医药大学,天津300193

出　　处：《中华中医药学刊》2009年第10期2079-2081,共3页Chinese Archives of Traditional Chinese Medicine

基　　金：教育部高等学校科技创新工程重大项目培育基金项目资助课题(706013)

摘　　要：目的:研究桑叶中1-脱氧野尻霉素(DNJ)的提取与精制工艺,建立1-脱氧野尻霉素(DNJ)的定性鉴别及含量测定方法。方法:本研究取桑叶药材,加70%乙醇提取,将提取液浓缩,通过大孔吸附树脂,取通过大孔吸附树脂的流出液,浓缩,通过阳离子交换树脂,用蒸馏水洗,用0.5mol/L氨水洗脱,收集洗脱液,浓缩,浓缩液通过硅胶纯化,将有杂质的组分弃去,合并含1-脱氧野尻霉素较纯的组分,浓缩,真空干燥,即得1-脱氧野尻霉素(DNJ)。1-脱氧野尻霉素的定性鉴别采用薄层鉴别法,吸取溶液点于薄层板上,展开剂为乙酸乙脂-无水乙醇(2:8),碘熏法进行显色,置紫外光灯(254nm)下检视。供试品色谱中,在与对照品色谱相应的位置上,显相同颜色的荧光斑点。1-脱氧野尻霉素的含量测定采用柱前衍生化高效液相色谱法,以芴甲氧羰酰氯(Fmoc-Cl)作为衍生化试剂,在pH=8.5硼酸盐缓冲液中进行衍生化反应后,生成具有紫外吸收的DNJ-FMOC络合物,用反相高效液相色谱—紫外检测法分离测定DNJ-FMOC。采用十八烷基硅烷键合硅胶色谱柱;流动相为乙腈-0.1%冰醋酸(11:16);检测波长为254nm。结果:经测定1-脱氧野尻霉素的含量为23.2%,收率为0.355%。结论:本方法工艺流程简单、快速、收率及含量高,适合于工业生产。Objective：To extract and purify DNJ from Morus alba L. Methods：The mulberry were prepared by the process of boiling with 70 percent ethanol and condensing. The concentrated extract flew the D101 type macroporous resin. The concentrated outflow is separated by 732 H type resin cation, cleansed by ammonia water（0.5mol/L）. The concentrated outflow is purified by silica. Results： In this way,the purity exceeded 23.2%, the yield could attain 0. 355%. Conclusion：This method is advantageous for its simple technical process, high speed, high yield and the purity. It is suitable for the industrialization.

关 键 词：桑叶 1-脱氧野尻霉素 阳离子交换树脂 硅胶 提取 精制 

分 类 号：R284.2[医药卫生—中药学]