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基于混合模式表面静电排斥/反相色谱法的[某物质]生物碱分析方法

[An analytical method for alkaloids of based on mixed-mode surface electrostatic exclusion/reversed-phase chromatography].

作者信息

Zhang Huarong, Guo Zhimou, Yu Wei, Yan Jingyu, Jin Gaowa, Wang Lianzhi

机构信息

Hubei University for Nationalities, Enshi 445000, China.

Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China.

出版信息

Se Pu. 2018 Oct 8;36(10):1053-1060. doi: 10.3724/SP.J.1123.2018.06006.

Abstract

A mixed-mode chromatographic method based on surface electrostatic exclusion and reversed-phase chromatography was established for the determination of alkaloids present in . The effects of two mobile phase additives, formic acid and acetic acid, on retention, peak shape and selectivity of the alkaloids in 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 . The main chromatographic peaks of 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 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 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.

摘要

建立了一种基于表面静电排斥和反相色谱的混合模式色谱方法,用于测定[具体物质]中存在的生物碱。使用自制的C18HCE柱,研究了两种流动相添加剂甲酸和乙酸对[具体物质]中生物碱保留、峰形和选择性的影响。发现以0.1%(v/v)的乙酸作为添加剂最有利于有效分离[具体物质]中存在的主要生物碱。通过所建立的方法和参考文献识别出[具体物质]的主要色谱峰,分别为黄连碱、表小檗碱、非洲防己碱、药根碱、小檗碱和巴马汀。参照2015年版药典中[具体物质]的含量测定方法,小檗碱在0.5 - 100 mg/L范围内线性关系良好,相关系数为0.9996,平均回收率为93.74%。测定了湖北和重庆不同批次[具体物质]中生物碱的含量。该方法简便、可靠、准确,可为其他碱性化合物的分离分析提供参考。

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