【作者】 武晓云；

【导师】 郭海蓉；

【作者基本信息】 广西大学 ， 制糖工程， 2007， 硕士

【摘要】 植物甾醇具有保持生物内环境稳定、控制糖原和矿物质的代谢、调节应激反应等十分重要的生理功能，有很高的应用价值，被誉为“生命的钥匙”。由于属于天然物质、本身无毒性，而且具有乳化性和稳定性等特点，因此引起各国科学家对植物甾醇开发应用的重视，因各自的结构、功能、以及医用合成需求不同，甾醇单组分分离富集的工艺研究也具有很实际的意义。本文采用分步法和一步法两种工艺方法从甘蔗糖厂滤泥中提取植物甾醇，并对得到的植物甾醇进行精制，进而分离富集豆甾醇和β-谷甾醇。论文首先对植物甾醇的提取分离、精制以及分析方法进行了比较系统地论述和探讨，综合各方面条件，选用皂化法对植物甾醇进行提取、选用溶剂重结晶法对植物甾醇进行精制研究。设计正交试验对各影响因素和条件进行筛选，找到从甘蔗糖厂滤泥中提取、精制植物甾醇以及从高纯度植物甾醇中分离富集豆甾醇和β-谷甾醇的最适工艺条件。同时对实验所得植物甾醇产品的皂化值、酸值、含皂量等性质做了测定，并用红外、气质联用光谱对其组成成分和相对含量进行了检测分析。用分步法提取植物甾醇，对干滤泥的得率为8.4‰～15.5‰，酒精回收率在70％左右，石油醚的回收率接近70％。而采用一步法提取植物甾醇，植物甾醇得率只能达到8.7‰，酒精回收率约为66.7％，石油醚的回收率在75％左右。实验发现，一步法工艺流程不仅大大缩短了工作周期，同时节约了化学溶剂，减轻了环境压力。实验所得植物甾醇粗品的相对含量达到56.34％，以正己烷为溶剂，在5℃条件下养晶1h对植物甾醇进行精制，精制植物甾醇的得率约为50％～60％，相对含量能达到96.59％。经GC-MS分析表明，精制植物甾醇主要成分为豆甾醇、β-谷甾醇和菜油甾醇，占挥发物的92.40％，另外，还有少量的麦角甾醇、γ-谷甾醇以及一些脂肪醇、烷烃、烯烃和酯等。实验以正戊醇为溶剂，采用重结晶法从精制植物甾醇产品中分离富集豆甾醇，用1：5的料液比(g／mL)，经过四次重结晶后，豆甾醇的相对含量达到86.93％，得率为15.19％。以环己酮为溶剂，采用分级结晶法从精制植物甾醇产品中分离富集β-谷甾醇，用1：4的料液比(g／mL)，经过三次分级结晶后，β-谷甾醇的相对含量可达到67.85％，得率为7.04％。更多还原

【Abstract】 Phytosterols is considered as "The key to life " because of its importantphysiology functions such as keeping the environment inside the living creaturestable, controlling the metabolism of sugar and mineral materials, regulatingstress reaction and so on. Belonging to natural materials, having no poison,having characteristics such as emulsibility and stability, etc cause scientists fromall countries to take a high value of the development and application ofphytosterols. Because of the differences in structure, function, need of medicalsynthesis, technological research on the separation and enrichment ofone-component phytosterol has practicable significance.Two kinds of craft methods including fractional steps method and one-stepmethod were adopted in this paper to extract phytosterols from filter mud ofsugarcane factory, in the subsequent handling, phytosterols was purified, thenstigmasterol andβ-sitosterol were separated and enriched from phytosterols withhigh purity.The methods of extracting, refining and analysing phytosterols were discussed and probed into systematically, considering all aspects and conditions,the saponification method was selected to extract, the recrystallization methodwas selected to refine phytosterols in this research. Orthogonal test was designedto screen out the optimum technological conditions of extracting phytosterolsfrom filter mud of sugarcane factory, refining phytosterols from crude product,seperating and enriching stigmasterol andβ-sitosterol from phytosterols withhigh purity. In the meantime, the properties of phytosterols such assaponification value, acid value, content of soap were analyzed, the compositionand relative content were determined by Infra-red spectrum and GC-MSspectrum.Using fractional steps method, the yield of phytosterols to filter mud is 8.4‰-15.48‰, the recovery rate of alcohol is about 70% and that of petroleumether is close to 70%. Using one-step method, the yield of phytosterols to filtermud was 8.7‰, the recovery rate of alcohol is about 66.7% and that ofpetroleum ether is about 75%. One-step method technological process could notonly shorten the work cyclic, but also economize the chemistry solvents, easethe pressure of environment.The relative content of crude phytosterols gained in this experimentreached up to 56.34%, Using n-hexane as sovent, crude phytosterols wascultured one hour under 5℃, the relative content of the refined phytosterolsreached up to 96.59% while the yield was 50%～60%. The result of GC-MSanalysis showed that refined phytosterols was mainly consist of stigmasterol, β-sitosterol and campesterol, whose relative cotent could reach up to 92.40%,except this, there were still a little amount of ergosterol,γ-sitosterol, some otherkinds of fatty alcohols, alkanes, alkenes, etc.Using n-pentanol as solvent, 1:5 as the ratio of phytosterols to thesolvent(g/mL), after being recrystallized four times, stigmasterol whose relativecotent was 86.93%, while the yield was 15.19%, was separated and enrichedform refined phytosterols products by recrystallization method. Usingcyclohexanone as solvent, 1:4 as the ratio of phytosterols to the solvent(g/mL),after three times of fraction crystallization,β-sitosterol whose relative cotentwas about 67.85%, while the yield was 7.04%, was separated and enriched formrefined phytosterols products by fraction crystallization method.更多还原