基于表面静电排斥/反相混合模式色谱的黄连生物碱分析方法  

An analytical method for alkaloids of Coptis chinensis based on mixed-mode surface electrostatic exclusion/reversed-phase chromatography

作　　者：张华蓉 郭志谋[2,3] 于伟 闫竞宇 金高娃[2,3] 王联芝 ZHANG Huarong;GUO Zhimou;YU Wei;YAN Jingyu;JIN Gaowa;WANG Lianzhi(Hubei University for Nationalities,Enshi 445000,China;Dalian Institute of Chemical Physics,Chinese Academy of Sciences,Dalian 116023,China;DICP-CMC Innovation Institute of Medicine,Taizhou 225300,China)

机构地区：[1]湖北民族学院,湖北恩施445000 [2]中国科学院大连化学物理研究所,辽宁大连116023 [3]中科院大化所中国医药城生物医药创新研究院,江苏泰州225300

出　　处：《色谱》2018年第10期1053-1060,共8页Chinese Journal of Chromatography

基　　金：中科院大化所中国医药城生物医药创新研究院首期建设经费;国家自然科学基金项目(21505131)~~

摘　　要：建立了基于表面静电排斥/反相混合模式色谱的黄连生物碱分析方法。选用实验室自制的C18HCE柱,以乙腈和水为流动相,考察了甲酸、乙酸两种流动相添加剂及其在流动相中的体积分数对黄连生物碱的保留、峰形及选择性的影响。最终确定0. 1%(v/v)乙酸作为添加剂能实现黄连生物碱的良好分离,结合质谱和文献对其主要色谱峰进行了识别,分别为黄连碱、表小檗碱、非洲防己碱、药根碱、小檗碱、巴马汀。参考2015版《中国药典》对黄连生物碱的含量测定方法,以盐酸小檗碱进行方法学考察,结果表明,在0. 5~100 mg/L范围内线性关系良好,相关系数为0. 999 6,平均加标回收率为93. 74%。利用所建立的方法测定了湖北和重庆两个产地不同批次的黄连样品中各生物碱的含量。该方法简便,重复性好,精密度高,可为其他碱性化合物的分离分析提供参考。A mixed-mode chromatographic method based on surface electrostatic exclusion and reversed-phase chromatography was established for the determination of alkaloids present in Coptis chinensis. The effects of two mobile phase additives, formic acid and acetic acid, on retention, peak shape and selectivity of the alkaloids in Coptis chinensis were investigated using the self-made C18HCE column. Acetic acid （0.1%, v/v） used as the additive was found to be optimum for effective separation of the main alkaloids present in Coptis chinensis. The main chromatographic peaks of Coptis chinensis were recognized by the established method and references, which were coptisine, epiberberine, columbamine, jatrorrhizine, berberine and palmatine, respectively. With reference to the content determination method of Coptis chinensis in the 2015 edition of pharmacopoeia, the linear relationship of berberine in the range of 0.5-100 mg/L was good, the correlation coefficient was 0.9996, and the average recovery was 93.74%. The contents of alkaloids in Coptis chinensis in different batches of Hubei and Chongqing were determined. The method is simple, reliable and accurate, and can be used as reference for separation and analysis of other basic compounds.

关 键 词：静电排斥/反相混合色谱模式 生物碱 黄连 峰形 选择性 

分 类 号：O658[理学—分析化学]