pH区带精制逆流色谱法分离制备黄藤中巴马汀和药根碱  

Separation and Preparation of Palmatine and Jateorhizine in Fibraurea recisa Pierre. by pH-Zone-Refining Counter-Current Chromatography

作　　者：井凤[1] 耿岩玲[1] 刘伟[1] 段文娟[1] 王岱杰[1] 王晓[1] 

机构地区：[1]山东省中药质量控制技术重点实验室山东省分析测试中心,济南250014

出　　处：《天然产物研究与开发》2016年第12期1943-1946,共4页Natural Product Research and Development

基　　金：山东省科技发展计划(2014GZX219003);山东省三院联合专项(ZR2016YL006)

摘　　要：建立了黄藤生物碱快速分离制备的pH区带精制逆流色谱方法。采用95%乙醇加热回流提取制备黄藤生物碱粗提物,利用pH区带精制逆流色谱法对生物碱粗提物进行直接分离制备,以氯仿-甲醇-水(4∶3∶3)为溶剂系统,下相添加三乙胺(10 mmol/L)为流动相,上相加盐酸(40 mmol/L)作为固定相,在主机转速800 rpm,流动相流速2 m L/min,检测波长254 nm条件下进行分离制备。从1.5 g黄藤提取物中一次分离得到231.6 mg药根碱和436.8 mg巴马汀,纯度均大于98%。化合物通过MS、~1H NMR和^(13)C NMR进行了结构鉴定。pH区带精制逆流色谱法是一种快速高效的分离纯化黄藤生物碱的方法。A rapid method was developed for the preparative separation of alkaloids from Fibraurea recisa Pierre. by pH- zone-refining counter-current chromatography. The crude sample was prepared by 95% ethanol reflux extraction and direedy separated by pH-zone-refining counter-current chromatography. The solvent system was chloroform-methanol-water （4： 3：3 ,v/v） with 40 mM HCI in the upper stationary phase and 10 mM TEA in the lower mobile phase. The rotation speed was set at 800 rpm. The flow rate was 2.0 mL/min and the detective wavelength was 254 nm. From 1.5 g of the crude sample,231.6 mg of jatrorrhizine and 436.8 mg of palmatine were obtained and each with a purity higher that 98% as determined by HPLC. The chemical structures were identified according to MS ,^1H NMR and ^13C NMR, The pH- zone-refining counter-current chromatography was a rapid and efficient method for the separation of alkaloids from Fibraurea recisa Pierre.

关 键 词：黄藤 pH区带精制逆流色谱 生物碱 药根碱 巴马汀 

分 类 号：R284.2[医药卫生—中药学]