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1、·摘要本文研究了從廢次煙葉中提取、純化茄尼醇的工藝,該工藝包括茄尼醇的提取,粗萃物的皂化和茄尼醇粗品的提純。首先建立了一種能較準(zhǔn)確測(cè)定煙葉中游離茄尼醇含量的方法,并以此法測(cè)定了各種煙葉中游離茄尼醇的含量,結(jié)果表明:廢次煙葉中的游離茄尼醇含量?jī)H略低于上等煙葉,煙梗也較具有提取價(jià)值。采用正相高效液相色譜法定量分析茄尼醇含量并建立了茄尼醇的薄層層析快速定性分析方法。其次研究了超臨界CO2流體萃取法和有機(jī)溶劑萃取法提取廢次煙葉中茄尼醇的工藝。單因素實(shí)驗(yàn)考察萃取過程各主要影響因素的基礎(chǔ)上,正交實(shí)驗(yàn)優(yōu)化得到了各自的較佳萃取工藝條件,在各自較佳工藝條件下分別進(jìn)行實(shí)
2、驗(yàn)得出:超臨界CO2流體萃取法所得茄尼醇的提取率為1.28%,得率為:92.1%;有機(jī)溶劑萃取法所得茄尼醇的提取率為1.25%,得率為:90%。結(jié)果表明:超臨界C02流體萃取法與有機(jī)溶劑萃取法相比具有溶劑消耗量少、萃取時(shí)間短、對(duì)茄尼醇的提取率高等優(yōu)點(diǎn),更適合于提取廢次煙葉中的茄尼醇。確立了茄尼醇粗萃物的皂化工藝條件,皂化液經(jīng)水洗、稀鹽酸中和、分層,茄尼醇含量可達(dá)52.6%。最后研究了兩種茄尼醇粗品純化工藝。經(jīng)100-200目硅膠柱吸附,不同濃度的石油醚-丙酮混合液梯度洗脫,丙酮重結(jié)晶,真空干燥,茄尼醇純度由52.6%提高到了93.5%,達(dá)到了制藥的純
3、度要求,該工藝過程簡(jiǎn)單,純化效果好;探索了分步重結(jié)晶法純化茄尼醇粗品的新工藝:皂化后茄尼醇粗品經(jīng)丙酮、甲醇、乙腈分步重結(jié)晶,真空干燥,獲得了含量為90.5%的茄尼醇精品。該法較現(xiàn)有提純方法具有所用設(shè)備簡(jiǎn)單、可操作性強(qiáng)、成本低、易于工業(yè)化等優(yōu)點(diǎn),此項(xiàng)技術(shù)對(duì)于高純度茄尼醇的工業(yè)化生產(chǎn)具有一定的指導(dǎo)意義。關(guān)鍵詞:茄尼醇;萃取工藝;提純;煙葉;重結(jié)晶Ⅰ····ABSTRACTTheextractionandpurificationofsolanesolfromdiscardedtobaccoleaveswerestudied.Theprocessinclud
4、essolanesolextraction,rudeextractssaponification,andrudesolanesolpurification.First,amoreaccuratedeterminationmethodoffreesolanesolindiscardedtobaccoleaveswasfound.Contentoffreesolanesolinvarioustobaccoleaveswasdeterminatedwiththismethod.Theresultsshowed:Freesolanesolcontentind
5、iscardedtobaccoleaveswasonlyslightlylowerthaninthefirst-classtobaccoleaves,Thetobaccopedunclesalsohadvalueinuse.Atthesametime,Straight-phaseHLPCwasusedforquantitativedeterminationofthefreesolanesolcontentandTLCwasfoundforfastqualitativeanalysisofsolanesol.Secondly,itwasinvestig
6、atedthatuseofsupercriticalcarbondioxidefluidextractionprocessandorganicsolventsextractionprocessfortheextractionofsolanesolindiscardedtobaccoleaves.OnthebasisofSingle-factorexperimentsinspectionoftherespectivemainfactorsinfluencingextractionprocess,therespectiveoptimalextractio
7、nconditionswereobtainedbyorthogonaloptimizedesign.Undertheirrespectiveoptimalextractionconditions,theextractionyieldofsolanesolwith1.28%wasobtainedin92.1%yieldbysupercriticalcarbondioxidefluidextractionmethodandtheextractionyieldofsolanesolwith1.25%in90%yieldbyorganicsolventext
8、ractionmethod.Theresultsshowed:comparedwithorganicsolv