红景天注射液的提取与精制工艺研究.docVIP

红景天注射液的提取与精制工艺研究 作者：杨婷媛 李三鸣 刘洪卓 姚慧敏 李红菊 【关键词】 红景天注射液 提取 精制 红景天苷 酪醇 　　Abstract：ObjectiveTo study the extraction and purification process of Hongjingtian Injection. MethodsAn orthogonal method was adopted to optimize the extraction and purification process with the transference rate of Salidroside and p-Tyrosol as criterion. ResultsThe optimized process of extraction was that eight times water as extracted solvent, the comminuted medical material was extracted three times，each for an hour. Alcohol precipitation method and gel flocculating method were both used to optimize purification process. Alcohol precipitated concentration was 70%. The optimized process of gel flocculating method was that the extracted solution was condensed to 0.5g·ml-1 (equivalent to raw materia1) and its pH was adjusted to 5.0. The 5.0% gelatin solution was added into the condensed solution with agitation rate of 60 r·min-1 at 60℃ until there was no more precipitation. ConclusionThe results of impurity test meet the standard for injection. The established methods can be used for extraction and purification of Hongjingtian injection. 　　Key words：Hongjingtian Injection; Extraction; Purification; Salidroside; P-Tyrosol 　　红景天为景天科植物红景天的干燥根和根茎，性寒，味微苦、涩，临床上常以水煎入药，具有清热解毒、活血化淤之功效。现代研究表明，红景天对心脑血管疾病具有很强的治疗作用，且无明显的毒副作用，有着极好的应用前景。中药输液与小针剂相比，在不溶性微粒控制、有关物质检查、提高有效成分分析方法检测方面均具有更高的灵敏度与准确度，同时又避免了小针剂配伍中可能引起的不良反应，虽然在制剂难度上很大，但在临床使用的安全有效性和产品的可控性等方面却都起到了“质”的变化［1］。红景天苷和酪醇［2,3］是红景天中已知的两种活性成分，本文以红景天苷和酪醇的总转移率为指标，对红景天注射液的提取与精制工艺进行研究。 　　1 仪器与试药 　　LC-10ATVP高效液相色谱仪，日本岛津株氏会社；RE-52A旋转蒸发仪，上海亚荣生化仪器厂；微型植物试样粉碎机，天津泰斯特仪器有限公司；DF-101S 集热式恒温加热磁力搅拌器，巩义市英峪予华仪器厂。 　　红景天，产地西藏；红景天苷对照品，购自中国药品生物制品检验所；酪醇对照品，购自日本；乙腈、甲醇均为色谱纯；水为二次蒸馏水；其他试剂均为分析纯。 　　2 方法与结果 　　2.1 红景天苷和酪醇的HPLC分析条件 色谱柱：ODS(Kromasil C18，250 mm×4.6 mm，5 μm，天津科技仪器有限公司)；流动相为甲醇-乙腈-0.06%磷酸（10∶10∶80,v/v/v），流速1.0 ml·min-1，检测波长275 nm，进样量20 μl。 　　2.2 提取工艺的研究 　　2.2.1 提取溶剂的选择考察了以水和不同浓度的乙醇作为提取溶剂，结果表明提取效果并没有显著差异，所以确定为以水作为提取溶剂。 　　2.2.2 提取工艺的优化取