葉安義Yeh, An-I臺灣大學:食品科技研究所何俊宏Ho, Chun-HungChun-HungHo2010-05-112018-06-292010-05-112018-06-292009U0001-1308200921272800http://ntur.lib.ntu.edu.tw//handle/246246/182214摘 要 山藥(Dioscorea spp.)是台灣常見的食物，含有許多對人體有益的生理活性成分，同時也是許多藥品及健康食品的原料，目前文獻中萃取山藥活性成分的方法多是使用有機溶劑(例如：甲醇、乙酸乙酯、石油醚)，若要作為藥物或食品的原料將面臨溶劑殘留與溶劑回收處理的問題。本研究主要目的為建立超臨界二氧化碳(SC-CO2)萃取山藥生理活性成分的方法，以熱力學公式計算出超臨界二氧化碳與山藥中活性成分的溶解度係數(solubility parameter)。分別以32、42、52oC 三種溫度；4000、3000、2000 psi 三種壓力進行超臨界萃取，觀察不同溫度、壓力與溶解度係數之超臨界流體對不同山藥活性成分之萃取效果，並與有機溶劑萃取產物比較，以探討兩者萃取物活性成分之差異性。 超臨界二氧化碳之溶解度係數影響其萃取之產物，高溶解度之SC-CO2 與有機溶劑皆對薯蕷皂配基(diosgenin)溶解度較高，低溶解度係數之SC-CO2 與有機溶劑則對植物固醇(stigmasterol, β-sitosterol)溶解度較高。溶解度係數受溫度與壓力改變影響，於固定壓力下溫度每上升10oC 溶解度係數則減少4.4-13%，固定溫度時壓力每上升1000 psi溶解度係數增加4.6-17.5%。Abstract　Dioscorea spp. is a kind of common food and material for drug and health food in Taiwan. There are many scholars studied about biological active compounds of Dioscorea spp., and most of them get the compounds by using solvent extraction. Supercritical fluid (SCF), at the temperature and pressure above critical point, material will exhibit properties different from gas and liquid at the supercritical state and we can change the physical properties of SCF by control the temperature and pressure. Carbon dioxide has been widely used as the solvent for supercritical extraction due to its safety and availability. Solubility parameter (δ) provides a numerical estimate of the degree of interaction between materials, and can be a good indication of solubility. The objective of this study is to investigate the feasibility of extracting bioactive compounds from yam using supercritical carbon dioxide. The operating conditions, temperature, pressure and solubility parameter, will be studied. Organic solvent and supercritical carbon dioxide extraction shows similar results, High solubility parameter organic solven and SC-CO2 can extract more diosgenin, and low solubility parameter organic solven and SC-CO2 can extract more phytosterol (stigmasterol, β-sitosterol). Theolubility parameter of supercritical carbon dioxide will be affect by changing pressure and temperature. It decreases 4.4-13%/10oC at fixed pressure and increases 4.6-17.5%/1000 psi at fixed temperature.目 錄次要................................................................................................................Ibstract.........................................................................................................II、前言........................................................................................................1.　背景........................................................................................................12.　實驗目的..............................................................................................3、文獻整理................................................................................................4.　山藥..................................................................................................4 1.1　簡介..........................................................................................4.2　一般成分與生理活性成分............................................81)一般成分..............................................................................82)活性成分..............................................................................9. 多醣.........................................................................9. 皂素.........................................................................9. 植物固醇................................................................10.　超臨界二氧化碳萃取技術............................................................13.1　超臨界流體之簡介................................................................13.2　超臨界流體之基本性質........................................................16.3 二氧化碳流體之特性............................................................22.4　超臨界二氧化碳萃取之應用與研究....................................24.　溶解度係數....................................................................................27.1 超臨界二氧化碳之溶解度係數............................................28.2 活性成分之溶解度係數........................................................31、材料與方法..........................................................................................38.　實驗材料........................................................................................38. 實驗藥品與溶劑............................................................................39(1) 標準品..............................................................................392) 溶劑..................................................................................39. 實驗儀器........................................................................................40. 實驗架構........................................................................................43. 實驗方法........................................................................................441) 液相層析法......................................................................44 . 高效能液相層析條件...........................................44. 薯蕷皂配基與植物固醇之定量...........................442) 溶劑萃取法......................................................................443) 超臨界二氧化碳萃取......................................................45. 不同二氧化碳流量之超臨界萃取.......................45. 不同溫度之超臨界萃取.......................................46. 不同壓力之超臨界萃取.......................................464) 液相層析分析樣品前處理..............................................47、結果與討論..........................................................................................49. 檢量線..............................................................................................49. 基隆山藥基本成分分析..................................................................52. 溶解度係數......................................................................................531) 超臨界二氧化碳之溶解度係數......................................532) 山藥活性成分之溶解度係數..........................................54. 液相層析........................................................................................591) 經酸水解與皂化處理過之樣品分析結果......................59. 超臨界二氧化碳萃取......................................................................651) 二氧化碳流量對超臨界萃取之影響..............................652) 溫度對超臨界萃取之影響..............................................653) 壓力對超臨界萃取之影響..............................................73、結論.....................................................................................................79、符號表...........................................80、參考文獻.........................................81、附錄......................................................................................................92 目 錄次一、各品種山藥外觀................................................................................7二、純物質之典型壓力對溫度相圖......................................................14三、對比壓力與對比密度之關係圖......................................................19四、二氧化碳於不同溶劑能力下之應用..............................................25五、超臨界二氧化碳於不同溫度、壓力下之溶解度係數..................30六、超臨界萃取裝置圖..........................................................................41七、液相層析法分析山藥植物固醇及薯蕷皂配基之分析流程..........48八、薯蕷皂配基與植物固醇標準品之分析圖譜..................................60九、(A)甲醇、(B)乙酸乙酯與(C)超臨界二氧化碳於32oC、4000 psi條件下之萃取物經酸水解與皂化後之液相層析圖譜.....................61十、在固定壓力4000psi於不同溫度下之超臨界二氧化碳萃取物經酸水解與皂化後之分析圖譜.................................................................63十一、在固定溫度32oC於不同壓力下之超臨界二氧化碳萃取物經皂化與水解後分析圖譜.........................................................................64十二、凍乾山藥粉末於32oC, 4000 psi 不同CO2流量的萃取率.....66十三、凍乾山藥粉末於CO2流量5 NL/min, 4000 psi 不同溫度的萃取率.........................................................................................................68十四、薯蕷皂配基萃取量與溫度變化之關係圖.................................70十五、植物固醇stigmasterol萃取量與溫度變化之關係圖................71十六、植物固醇β-sitosterol萃取量與溫度變化之關係圖..................72十七、凍乾山藥粉末於CO2流量5 NL/min，溫度32oC下不同壓力的萃取率.................................................................................................73十八、薯蕷皂配基萃取量與壓力變化之關係圖..................................76十九、植物固醇stigmasterol萃取量與壓力變化之關係圖.................77二十、植物固醇β-sitosterol萃取量與壓力變化之關係圖...................78 目 錄次一、不同流體狀態下之基本物理性質..................................................17二、不同流體之臨界溫度與壓力..........................................................21三、液態二氧化碳之溶劑性質..............................................................23四、超臨界二氧化碳之優點..................................................................26五、一級結構之溶解度係數..................................................................33五、一級結構之溶解度係數(續)...........................................................34六、二級結構之溶解度係數..................................................................35七、δp和δhb低於3MP1/2時之一級結構溶解度係數...........................36八、δp和δhb低於3MP1/2時之二級結構溶解度係數...........................37九、植物固醇與薯蕷皂配基以210nm紫外光檢測器之線性迴歸方程式.........................................................................................................50十、甲醇、乙酸乙酯以及超臨界二氧化碳萃取物之活性成份含量.51十一、基隆山藥基本成分分析………………………………………..52十二、超臨界二氧化碳各種溫度壓力下之溶解度係數……………..53十三、薯蕷皂配基溶解度係數………………………………………..56十四、Stigmasterol溶解度係數.............................................................57十五、、β-sitosterol溶解度係數..............................................................58十六、不同超臨界二氧化碳流量之萃取量..........................................67application/pdf1925831 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