【作者】 薛绍玲；

【导师】 凌敏；

【作者基本信息】 广西大学 ， 林产化学加工工程， 2007， 硕士

【摘要】 本文采用水逆流连续浸提栀子苷，用现代膜分离技术对栀子粗提液进行预处理，然后采用大孔树脂吸附法和双水相萃取法两种不同的工艺分离纯化栀子中栀子苷，最后对从纳滤透过液中回收栀子苷的工艺进行了研究。所有实验均进行了放大实验研究，为栀子苷的工业化生产提供理论依据。在分离纯化前对传统的栀子浸提工艺进行改进，以水作为浸提溶剂替代了传统的乙醇浸提，采用多级逆流浸提方式代替传统的单罐间歇式浸提。运用正交实验法确定了水浸出法在室温时浸出条件：栀子粉碎度40目；浸出次数3级；液料比4：1，在此条件下栀子苷的浸出率为85.28％。原料预处理中采用陶瓷膜微滤技术和纳滤浓缩技术对浸提液进行澄清和浓缩替代传统的过滤和蒸发浓缩，从而得到栀子苷含量为48mg／mL的优质原料液。X-5型大孔树脂吸附分离栀子苷分离纯度高达85％以上，吸附柱可按比例放大进行工业化生产。吸附量大，每150g树脂可吸附栀子苷48mg／mL的栀子原料液500mL，而且洗脱方法简单，溶剂量消耗少，吸附饱和的150g树脂采用10％的乙醇5000mL可将大部分栀子苷洗脱下来，然后用50％到70％的乙醇进行梯度洗脱可以将色素全部洗脱下来。双水相萃取法生产周期短，一次性处理量大，可应用于工业生产中栀子苷的粗分离，增加盐的浓度或者减少PE62的浓度，将导致萃取分离效率的增加，当系统条件是含5％的PE62，10％的KH₂PO₄和10％的乙醇添加量时分离效果最佳，在最佳条件下栀子苷的收率可达到89.9％。直接用大孔吸附树脂D101富集回收纳滤透过液中栀子苷的方法简便易行，回收效率高。当原液浓度为0.5mg·mL^-1、流速为5mL·min^-1时，树脂对栀子苷的吸附效果最好。树脂吸附栀子苷以后，从吸附效率、节能、省时等角度考虑，洗脱流速为10mL·min^-1，洗脱液为70％乙醇最佳。更多还原

【Abstract】 In this paper, the conventional producing technology of geniposide waschecked and modified. Multilevel counter-flow extraction was used to extractgeniposide from gardenia fruit. Then modem membrane separation technologywas used to pretreat the crude solution. Macroporous resin adsorption andaqueous two-phase extraction was also used to separate and purify geniposide inthis paper. At last macroporous resin adsorption was used to reclaim geniposidefrom the permeating solution of nanofiltration. All tests had been magnified.Thus, this paper can afford conformity in theory for the industrializedproduction.Water was select as the extraction solution. The optimal condition ofmultilevel counter-flow extraction was determined by comparing with one potintermittently extraction. Orthogonal test method was used to study theinfluence of extraction degree, extraction period, extraction granularity, ratio ofliquid to material. The best conditions were to extract three times, every timeadded four times water into the crude and crushed the gardenia fruit into 40 meshes for half an hour.Through clarified by Ceramic micro-filter membrane and concentrated bynanofiltration, Good extraction liquid was gained and the content of roughgeniposide reached 48mg/mL.Macroporous resin adsorption of X-5 could purify the geniposide to above85%. It could adsorb 500mL extraction liquid for every 150g resin. Geniposideand yellow pigment can be washed respectively by 10%, 50% and 70% ethanol.This method was saving and convenient. It washed the great mass of geniposideonly with 5000mL ethanol of 10%. It could be magnified to produce geniposideat some proportion.Aqueous two-phase extraction could be used to separate mainly geniposidefrom gardenia fruit. Its production period was short. It could deal with a greatdeal of raw material at one time. The partition efficiency of geniposide could beenhanced by increasing salt concentration or decreasing PE62 concentration. Anoptimized system containing 5% PE62, 10% KH2PO4, and 10% ethanol wasdeveloped and shown to be effective for the extraction of geniposide fromgardenia fruit. Under the best condition the recovery yield of geniposide couldreach 86%.Resin D101 could be used to collect gardenoside from permeating solutionof nanofiltration directly, which was simple and convenient. When theconcentration of gardenoside was 0.5 mg·mL^-1 and the flow rate of absorptionwas 5 mL·min^-1, the effect of adsorption was the best. After the absorption, 70%ethanol was used to wash the geniposide at flow rate of 10 mL·min^-1 consider ofthe absorption efficiency, cost saving and time saving.更多还原