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首页> 外文期刊>RSC Advances >Preparative separation of alkaloids from Litsea cubeba using combined applications of pH-zone-refining and high-speed counter-current chromatography
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Preparative separation of alkaloids from Litsea cubeba using combined applications of pH-zone-refining and high-speed counter-current chromatography

机译：利用PH区炼油和高速反电流色谱法的组合应用，从Litsea CubeBA制备生物碱的分离

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摘要

Litsea cubeba is characterized by the presence of aporphine alkaloids. But few recent reports about the preparative separation of alkaloids from L. cubeba are found. The traditional separation method is time consuming and solvent consuming and irreversible adsorption is inevitable. In this research, pH-zone-refining counter-current chromatography and high-speed counter-current chromatography are applied to separate the alkaloids from a chloroform extract of L. cubeba. The crude extract was fractionated using the solvent system: chloroform-methanol-water (4 : 3 : 3, v/v) with different concentrations of hydrochloric acid (retainer) in the aqueous stationary phase and triethylamine (eluter) in the organic mobile phase to determine the ideal conditions for screening for the aporphine alkaloids. Using 1.5 g of the chloroform extract, 68.1 mg of norisocorydine (93.5% purity), 215.5 mg of isoboldine (96.3% purity), 612.3 mg of the mixture of boldine and laurotetanine, 108.8 mg of reticuline (97.4% purity) and 92.6 mg of laurolitsine (97.6% purity) were obtained with the selected conditions where 60 mM of hydrochloric acid was added to the stationary phase and 10 mM of triethylamine was used in the mobile phase. The mixture of boldine and laurotetanine was further separated using high-speed counter-current chromatography with a two-phase solvent system composed of ethyl acetate-methanol-water (4 : 1 : 5, v/v). Two alkaloids, laurotetanine (285.7 mg) and boldine (112.3 mg), were obtained from 500 mg of the mixture, in a one-step separation, with the relative purity of 94.8% and 96.2%, respectively. The purities of the isolated alkaloids were determined using high performance liquid chromatography and the chemical structures were confirmed using electrospray ionization-mass spectrometry, proton nuclear magnetic resonance (H-1-NMR) and carbon-13 (C-13)-NMR.
机译：Litsea CubeBA的特征在于存在间腺生物碱。但是，发现有关近期关于从L.CubeBA的生物碱的制备分离的报告。传统的分离方法是耗时，溶剂消耗和不可逆的吸附是不可避免的。在该研究中，施加pH区精制逆流色谱和高速逆流色谱以将生物碱与L. CubeBA的氯仿提取物分离。使用溶剂系统分级分级：氯仿 - 甲醇 - 水（4：3：3，v / v），在有机流动相中具有不同浓度的盐酸（保持器）和三乙胺（Eluter）确定筛选白血水性生物碱的理想条件。使用1.5g氯仿提取物，68.1mg诺里非炎（纯度为93.5％），215.5mg异丙籽（96.3％纯度），612.3mg摩尔和洛嘧丁酸盐的混合物，108.8mg近硅（97.4％纯度）和92.6毫克用选定的条件获得Laurolitsine（97.6％纯度），其中将60mM盐酸加入到固定相中，在流动相中使用10mM三乙胺。使用高速逆流色谱法进一步分离胆碱和桂替甘替甘醇的混合物，其具有由乙酸乙酯 - 甲醇 - 水（4：1：5，v / v）组成的两相溶剂系统。两种生物碱，月洛替丹林（285.7mg）和摩尔（112.3mg），在一步分离中从500mg的混合物中获得，相对纯度分别为94.8％和96.2％。使用高效液相色谱法测定分离的生物碱的纯度，使用电喷雾电离质谱法，质子核磁共振（H-1-NMR）和碳-13（C-13）-NMR确认化学结构。

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  • 来源
    《RSC Advances》 |2015年第92期|共7页
  • 作者

    Sun Changlei; Li Jia; Wang Daijie; Yu Jinqian; Wang Xiao; Huang Luqi;

  • 作者单位

    Shandong Univ Tradit Chinese Med Coll Pharm Jinan 250355 Shandong Peoples R China;

    Shandong Univ Tradit Chinese Med Coll Pharm Jinan 250355 Shandong Peoples R China;

    Shandong Acad Sci Shandong Anal &

    Test Ctr Key Lab TCM Qual Control Technol Jinan 250014 Shandong Peoples R China;

    Shandong Acad Sci Shandong Anal &

    Test Ctr Key Lab TCM Qual Control Technol Jinan 250014 Shandong Peoples R China;

    Shandong Univ Tradit Chinese Med Coll Pharm Jinan 250355 Shandong Peoples R China;

    China Acad Chinese Med Sci State Key Lab Breeding Base Dao Di Herbs Natl Resource Ctr Chinese Mat Med Beijing 100700 Peoples R China;

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  • 正文语种 eng
  • 中图分类 化学;
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