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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 screen a highly effective combination of rhubarb free anthraquinones components extraction and purification methods. Methods Rhubarb roots and rhizomes were extracted by ethanol ultrasound, ethanol reflux, mixed solvent ultrasound and alkali-soluble acid precipitation respectively. Each method aids with acidolysis or acidification prior to extraction. Chloroform extraction, alkali-soluble acid precipitation and methanol in order to remove non-standard components of the crude extract (impurities). High performance liquid chromatography-diode array detection was used to identify and quantify five anthraquinone-containing compounds. Results The content of total anthraquinone obtained by assisted acid hydrolysis extraction was significantly higher than that by acid-assisted extraction or acid-assisted extraction (P <0.05). The high purity anthraquinones were obtained by acid hydrolysis, ultrasonic extraction by ethanol, Chloroform extraction, alkali-acid precipitation and methanolysis to obtain high purity (> 96%) free total anthraquinone. Analysis of eight batches of rhubarb extracts showed good reproducibility of the process by sonication of ethanol in combination with the above purification procedure, with a coefficient of variation of 9.51% between batches. Conclusion This method is expected to be applied to the pharmaceutical industry to improve the quality of rhubarb-based traditional Chinese medicine preparations.