高速逆流色谱法分离制备博落回血根碱与白屈菜红碱  

Separation and Preparation of Sanguinarine and Chelerythrine from Macleaya cordata Root by High Speed Counter-Current Chromatography

作　　者：贾长青 马瑞 钱玺丞 王丹丹 郁建生[2] JIA Changqing;MA Rui;QIAN Xicheng;WANG Dandan;YU Jiansheng(College of Pharmacy,Tongren Polytechnic College,Tongren 554300,China;National Engineering Center for Veterinary Medicine in Nationalities,Tongren Polytechnic College,Tongren 554300,China;Guizhou Fanjingshan Agricultural High-tech Co.,Ltd.,Tongren 554300,China)

机构地区：[1]铜仁职业技术学院药学院,贵州铜仁554300 [2]铜仁职业技术学院民族中兽药国家地方联合工程中心,贵州铜仁554300 [3]贵州梵净山农业高科技股份有限公司,贵州铜仁554300

出　　处：《食品工业科技》2022年第1期39-46,共8页Science and Technology of Food Industry

基　　金：贵州省科技计划项目(NO.黔科合基础[2018]1422);铜仁市科技计划项目(NO.(2019)12-2)。

摘　　要：本文旨在建立一种使用常规高速逆流色谱技术分离制备高纯度博落回血根碱和白屈菜红碱的方法。通过分析型高速逆流色谱对六种溶剂体系进行快速筛选,确定以三氯甲烷-甲醇-0.2 mol/L盐酸水溶液(4:2:2,V/V/V)为两相溶剂体系并放大到制备型高速逆流色谱上,以上相为固定相,下相为流动相,流速8 mL/min,转速为455 r/min,进样量1000 mg,温度为25℃条件下分离制备博落回血根碱和白屈菜红碱。实验结果表明:此方法一次性能够从1000 mg博落回生物碱粗品分离得到博落回血根碱盐酸盐505 mg和白屈菜红碱盐酸盐435 mg。经超高效液相色谱(UPLC)检测,按照外标法计算,两者纯度分别为99.77%、99.73%。采用标准品对照法、1H NMR和13C NMR对目标产物进行了结构鉴定。分离所得产物的结构数据与文献一致。该方法具有后处理简单、成本低廉、分离产物纯度高、实用性强等特点,适用于血根碱和白屈菜红碱的大量制备。The aim of this study was to develop a method for the separation and preparation of high purity sanguinarine and chelerythrine by conventional high speed counter-current chromatography. After comparing six kinds of solvent protocols of analytical high speed counter-current chromatography(HSCCC), the two phase system of chloroform-methanol-0.2 mol/L hydrochloric acid aqueous solution(4:2:2,V/V/V) was finally chosen as the operating solvent of preparative high speed counter-current chromatography(HSCCC), in which the upper phase was used as the stationary phase and the lower phase was used as the mobile phase. Under the conditions of ratations speed of 455 r/min, lower phase flow rate of 8 mL/min, the injection volume of 1000 mg, the temperature of 25 ℃, sanguinarine and chelerythrine was separated and preparated on HSCCC. The results showed that 505 mg of sanguinarine chloride and 435 mg of chelerythrine chloride could be obtained from 1000 mg of crude Macleaya cordata alkaloid at one time by this method. According to the calculation of external standard method, the purity of them were 99.77% and 99.73% respectively determined by UPLC. The structure of the two target product was identified by comparison with standards, 1 H NMR and 13 C NMR. The structure data of the separated products were in agreement with the literature. The method is suitable for the mass preparation of sanguinarine and chelerythrine, because it has many advantages such as simple post-treatment, low cost, high purity of separation products and strong practicability.

关 键 词：高速逆流色谱 博落回 血根碱 白屈菜红碱 制备 

分 类 号：TS201.1[轻工技术与工程—食品科学]