异紫堇二酮的半合成转化及红景天中红景天苷、络塞维分离纯化的分析-中药学专业论文.docx

中文摘要本论文以异紫堇碱为原料，通过选择合适的氧化剂半合成转化为异紫堇二酮，对异紫堇二酮的半合成转化工艺进行了研究，确定了最佳的合成工艺路线和工艺条件，为进一步研究其体内外药理活性奠定了基础。并利用柱色谱技术对红景天中红景天苷、络塞维的分离制备工艺进行了研究，初步确定了最佳的柱色谱制备工艺。论文内容主要包括以下几个部分：1 本文综述了异喹啉类生物碱中原小檗碱类化合物的合成转化、构效关系和药理活性的研究进展，对不同的合成方法进行了概述，并对这一研究领域的发展前景和发展方向做出展望。2 利用弗瑞米自由基成功地将异紫堇碱转化为异紫堇二酮，并对该反应合成工艺路线和工艺条件进行筛选，得出了最佳的反应条件：pH值为10 的磷酸氢二钠溶液为反应介质；反应温度25 ℃；投料比（异紫堇碱∶弗瑞米自由基）=1∶2；反应时间12 h。在此反应条件下产率可达到50.0%,并通过多种波谱技术对合成异紫堇二酮的化学结构进行表征。其结果为进一步研究异紫堇二酮的药理活性奠定了基础。3 利用柱色谱技术，初步研究从红景天中分离纯化红景天苷、络塞维2 个化合物的分离条件和制备工艺：红景天药材经粉碎、乙醇回流提取、减压浓缩、烘干后，浸膏拌样上柱分离。红景天苷洗脱条件为：先经氯仿-甲醇20:1-8:1（v:v）梯度洗脱，再用氯仿-甲醇10:1（v:v）等度洗脱之后可得，经高效液相色谱检测纯度达90.0%。络塞维洗脱条件为：先经氯仿-甲醇16:1-4:1（v:v）梯度洗脱后，再用氯仿-甲醇8:1（v:v）等度洗脱之后可得，经高效液相色谱检测纯度达94.0%。关键词：半合成转化；原小檗碱；异紫堇二酮；弗瑞米自由基；红景天苷；络塞维ABSTRACTTheaimofthisthesiswastodevelopawayofsemi-synthetictransformationof isocoydionefromisocorydinebyusingaproperoxidant.Theconditionsofsynthesisand purificationwereoptimized.Theresultsprovidedthebasisofinvitroandinvivo experimentsforfurtherresearchofitspharmacologicalactivities.Thestudyalsoaimedat developingamethodforpreparationofsalidrosideandrosavinfromroserootbyusing column chromatography.Themain contents of this thesis include:Thesynthetictransformation,structure-activityrelationshipandpharmacological activityofprotoberberinecompounds,whichbelongtoisoquinolinealkaloids,arereviewed inthispaper.Also,differentsyntheticmethodsaresummarized.Thedevelopmentprospect and direction ofthis researchfield arelooked forward.ByactingwithFremy’sradical, the transformation method ofsemi-synthesizing isocorydione from the natural product of isocorydinewas established. Thefactors affecting the reactionyield were investigatedin details. Theoptimum reaction conditions were determined as follows: reactingfor12 h inthesolution ofsodium dihydrogen phosphate at pH10, the temperaturewasset at 25 ℃and themass ratio of isocorydine to Fremy’sradical was1:2. Under theoptimum conditions, theyield could reach 50.0%.Themolecularstructureof isocorydionewaselucidated byX-raysingle-crystal diffraction an