摘要
目的:建立胆木中短小舌根草苷、3-表短小舌根草苷、异常春花苷内酰胺和喜果苷的快速制备色谱方法。方法:胆木药材水提物经AB-8大孔树脂初步纯化后,以自动纯化系统快速分离,根据色谱图收集流出液,制备得到4种生物碱。色谱柱采用Waters Xbridge OBD C18色谱柱(19mm×150mm,5μm),流动相乙腈-水,流速10m L/min;另外采用UPLC进行纯度分析,QTOF/MS进行结构鉴定。结果:质谱法确定实验所得的4种单体分别是短小舌根草苷、3-表短小舌根草苷、异常春花苷内酰胺和喜果苷,UPLC面积归一化法其纯度分别为99.0%、93.0%、98.7%和90.2%。结论:此法简便易行,所得化合物纯度较高,适用于胆木药材标准品的制备。
Objective：To establish a fast preparative method for the preparation of four alkaloids from Nauclea officinalis by using auto purification system.Methods：The aqueous extract of Nauclea officinalis was isolated quickly after purifing preliminary by using AB-8 macroporous resin.The outflow was obtained according to the chromatogram,and four alkaloids were obtained after preparing with the determination conditions were as following：determination column was C18 column（19mm×150mm,5um）;the mobile phase was acetonitrile-water;determine wavelength was 220 nm;flow velocity was 10mL/min.The purity and construction were analyzed by using UPLC and QTOF/MS,respectively.Results：Four alkaloids from Nauclea officinalis were pumiloside,3-epipumiloside,strictosamide and vincosamide,and the purity of the four alkaloids were 99.0%（pumiloside）,93.0%（3-epi-pumiloside）,98.7%（strictosamide） and 90.2%（vincosamide） according to area normalization method of UPLC.Conclusion：This method is simple and convenient,which is suitable for the preparation of the standards of Nauclea officinalis.
出处
《中华中医药杂志》
CAS
CSCD
北大核心
2016年第2期463-466,共4页
China Journal of Traditional Chinese Medicine and Pharmacy
基金
国家自然科学基金项目(No.81160558)
海南省自然科学基金项目(No.310047)~~
