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1、浙江大學(xué)碩士學(xué)位論文大豆胚芽中異黃酮提取研究姓名:李珊珊申請(qǐng)學(xué)位級(jí)別:碩士專業(yè):化學(xué)工藝指導(dǎo)教師:任其龍20040201摘要Y。581532本文研究了從大豆胚芽中提取和純化總異黃酮的方法與工藝,包括總異黃酮的初步提取和異黃酮提取物的固體酸水解兩個(gè)主要過程。在火豆胚芽總異黃酮初步提取條件優(yōu)化實(shí)驗(yàn)中,以單因素實(shí)驗(yàn)方法優(yōu)化了四個(gè)影響因素:提取溫度、提取時(shí)間、溶劑用量、溶劑濃度。以胚芽中總異黃酮提取率和提取的選擇性為指標(biāo),確定60%乙醇為提取溶劑、提取溫度50。C、提取次數(shù)三次、每次提取的液固比為6:1、三次的提取時(shí)間分別為60mirl、10min、lOmin,三次總提取率為92%。在
2、異黃酮固體酸水解實(shí)驗(yàn)中,選擇南開大學(xué)化工廠的D72強(qiáng)酸性陽離子交換樹脂作為固體酸催化劑。經(jīng)過兩次固定床水解反應(yīng),染料木素、大豆黃素和黃豆黃素等三種異黃酮轉(zhuǎn)化率可達(dá)90%。實(shí)驗(yàn)研究了溫度、甲醇水配比、進(jìn)料配比以及接觸時(shí)間對(duì)游離型異黃酮轉(zhuǎn)化率的影響。結(jié)果表明,在實(shí)驗(yàn)溫度范同內(nèi)(60~70。C),溫度變化對(duì)gen[stein和glyciteJn影響較明顯,溫度升高轉(zhuǎn)化率增大;溫度變化對(duì)daidzein的轉(zhuǎn)化率影響不大;接觸時(shí)間越長(zhǎng),反應(yīng)的轉(zhuǎn)化率越高,并逐漸趨向平衡值;甲醇水配比為1:2有利于水解反應(yīng);溶劑比例增大,三種異黃酮轉(zhuǎn)化率都增大,溶劑比例增大到一定程度轉(zhuǎn)化率變化不明顯。異黃酮
3、精制過程中,探索了柱層析、溶劑萃取、溶劑沉淀等方法,最終異黃酮含量可達(dá)40%,對(duì)胚芽異黃酮收率50%左右。建立了總異黃酮的分析方法和游離態(tài)異黃酮的HPLC分析方法。關(guān)鍵詞:大豆異黃酮大豆胚芽提取水解反應(yīng)固體酸采綴作者、導(dǎo)師同意勿全文公布ABSTRACTAprocessforextractingandpurilyingisofhvonesfromsoybeangermwasstudiedinthiSpaper’.Theprocessincludesextractionoftotalisoilatonesandhydro]yzationofsoybeanisoilavonebyso
4、lidacideatalyet.IntheexperimentSofextractionoftotalisoflavones,fivefactorswereStudied:temperature,extractingtime.coneentrationofsolventandamountofS01vent.WiththeextractioneffiCiency0ftotaliSOFlavonesandtheselectivitYofextractionasstudytargets.theoptiumextractionconditionswereasfollowed:solve
5、nt60%ethan01.temperature50℃,solventvolumetosobeangermweight6:1,extractingfor3times.60min、lOmin、1OminrespectjtelY.Extractionel’fiCiencyoftotalisoftavonesWaSabout92%.Intheexperiments0ffixedbedprocess,soybeanisoilatone91UCOSidecanbehydrolyzedintoisoflavoneagluconewithmethanolinafixedbedfi1ledwi
6、thSOlidacidcatalyst(NankaiChemicalFactory,D72).ConversionofisollatonesiSabout90%。Theeffectoftemperatut’e,contacttime,concentrationofmethanolandproportionofsolventtomaterialoncentersionwasstudied.Theresultsshowthatenhancingtemperatureandprolongingthecontacttimearefavorofthereaction,andtherati
7、0ofmethanoltowateriSappropriately1:2.Duringtheprocessofrefiningofisoflavonesfromtheextraction,methodssuchaschromatogram,extraction,depositionwereresearched.ContentofisoflavonewasashighaS40%,andrecoverypercentofisofIavonebasedonsoybeangermwasabout50