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作 者:李会丽[1] 杜丽东[2] 史彦斌[1] 刘晖[1] 张晓云[1] 李琰[1] 倪京满[1] 任远[2]
机构地区:[1]兰州大学药学院,兰州730000 [2]甘肃中医学院甘肃省中药药理与毒理学重点实验室,兰州730000
出 处:《兰州大学学报(医学版)》2014年第3期62-70,共9页Journal of Lanzhou University(Medical Sciences)
基 金:Open Foundation of Key Laboratory of TCM Pharmacology and Toxicology of Gansu Province(ZDSYS-KJ-2013-005);Agricultural Biotechnology Research and Development Project of Gansu Province(GNSW-2013-14),China
摘 要:目的筛选一种高效组合的大黄游离蒽醌类成分的提取和纯化方法。方法通掌叶大黄根和根茎分别用乙醇超声、乙醇回流、混合溶剂超声和碱溶酸沉淀法提取。每种方法在提取之前辅助以酸解或酸化处理。氯仿萃取,碱溶酸沉淀和甲醇溶解依次除去粗提物中的非指标性成分(杂质)。高效液相色谱-二极管阵列检测用于鉴别和定量5种蒽醌指标性化合物。结果辅助酸水解的提取工艺所得的总蒽醌含量显著高于辅助以酸化处理或未经酸处理的提取工艺(P<0.05);高纯度的大黄蒽醌可通过酸水解,乙醇超声提取,结合氯仿萃取、碱溶酸沉淀和甲醇溶解来获得高纯度(>96%)的游离总蒽醌。对八批次的大黄提取物的分析显示,用酸水解并结合上述纯化程序的乙醇超声提取法能获得良好的工艺重现性,不同批次间的变异系数为9.51%。结论该方法期望被应用医药工业,提高以大黄为主体的中药制剂的质量。Objective To select an effectively combined extraction and purification procedure for free anthraquinones from Radix et Rhizoma Rhei.Methods Radix et Rhizoma Rhei (Rheum palmatum L.) was extracted by ethanol ultrasonication,ethanol reflux,mixed-solvent ultrasonication and alkali extraction methods.Each method was assisted with acidization and/or acid hydrolysis before solvent extraction.Chloroform extraction,alkali-solution,acid-isolation,and methanol dissolution were adopted to remove impurities in the later purification stage.HPLC-DAD was used to identify and quantify five marker anthraquinones.Results The total concentration of anthraquinones obtained by extraction procedure assisted with acid hydrolysis treatment were higher than those with acidization or without acidic treatment (p < 0.05).Higher purity (> 96.0%) of rhubarb anthraquinones can be obtained using ethanol ultrasonication combined with acid hydrolysis,chloroform extraction,alkali-solution and acid-isolation,and methanol dissolution processes.Eight batches of rhubarb extracts showed good reproducibility of the total anthraquinone content with an average 9.51% of RSD using the proposed procedure.Conclusion The combined procedure can hopefully be applied in medicinal industry and improve the quality of rhubarb-based preparations.
关 键 词:大黄 大黄蒽醌 组合式提取和纯化工艺 方法重现性
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