大孔吸附树脂对贯叶金丝桃中苯并二蒽酮类成分的富集.doc

大孔吸附树脂对贯叶金丝桃中 苯并二蒽酮类成分的富集 樊敏伟1，宋崎 1*，王冰1，宋英1，奚静芳1，王建新2 上海市中药研究所，上海 201203；2．复旦大学，上海 200032) [摘要]目的　考察大孔吸附树脂对贯叶金丝桃中苯并二蒽酮类成分的富集方法, 并确定工艺路线和参数工艺路线和参数该可为的大孔树脂精制工艺提供参考。aphthodianthrones in Hypericum perforatum L. with Macroporous Resin FAN Min-wei 1，SONG Qi 1*，WANG Bing1，SONG Ying1，XI Jing-fang1，WANG Jian-xin2 (1.Shanghai Institute of Chinese Meteria Medica Shanghai 201203； 2. Fudan University Shanghai 200032) [Abstract] Objective To study the enrichment of naphthodianthrones in Hypericum perforatum L. with macropotous resin , and define the refinement process and adsorption factor. Methods The refinement process and adsorption factor of the separation and purification of naphthodianthrones in Hypericum perforatum L. with macroporous resin were compared by static and dynamic adsorbing experiments. And the content of naphthodianthrones was developed as its quality standard, screening out the best refinement process and adsorption factor. Results The refinement process and adsorption factor of the enrichment of naphthodianthrones in Hypericum perforatum L. with macroporous resin are stable and feasible .Conclusion The enrichment method can offer information about the determination of refinement process of Hypericum perforatum L. with macroporous resin. [Key words] Hypericum perforatum L.; naphthodianthrones; macropotous resin; static adsorption; dynamic adsorption 贯叶金丝桃为藤黄科植物贯叶金丝桃Hypericum perforatum L. 的干燥地上部分。贯叶金丝桃的主要化学成分包括苯并二蒽酮类化合物, 如金丝桃素、、、、、、、、、]。、、。UV-2401PC；2.1.1供试品和对照品的制备 供试品溶液：取样品约0.1g，精密称定，至50ml棕色量瓶中，加甲醇40ml，超声处理（功率350W、频率35KHz）40分钟，放冷，加甲醇至刻度，摇匀，过滤。精密量取续滤液2ml，置10ml棕色量瓶中，加甲醇至刻度，摇匀。 对照品溶液：精密称取五氧化二磷减压干燥24h的金丝桃素对照品，加甲醇-吡啶(9:1)配制成每1ml含金丝桃素20μg的溶液，置棕色量瓶中，作为对照品储备液。 2.1.2测定方法 分别取供试品溶液和对照品溶液，以试剂作空白，照分光光度法（中国药典2005年版一部附录VB），在588nm波长处测定吸收度，计算，即得。 2.1.3线性范围的考察 分别精密量取对照品储备液1.0ml、2.0ml、4.0ml、6.0ml、8.0ml于10mlμg/ml范围内苯并二蒽酮类浓度与吸收度有良好的线性关系。 2.2大孔吸附树脂有机残留物检查 　照有机溶剂残留量测定法（中国药典2005年版二部附录VIII P 第二法（30m×0.25mm×0.25μm）260℃及300℃；载气为氮气，流速：2.0ml/min；顶空取样瓶加热条件：120℃加热15min。 2.2.2供试品和对照