臺灣博碩士論文加值系統

本研究以大陸進口的乾貨為原料，首先在索氏提取器中以乙醇為溶劑進行銀杏葉之提取，並配合實驗設計與迴歸分析找出最佳的溶劑提取條件；然後，提取濃縮液並以吸附性層析技術進行製備分離濃縮與純化。結果顯示，最佳的溶劑提取條件為70 %乙醇水溶液、160ml、3小時，粗提物的黃酮類含量為2.5 %，內酯類含量為0.3 %；再經過轉溶程序後，黃酮類含量提高至4.9 %，內酯類含量提高至1.3﹪最後再經XAD7樹脂管柱以10 %乙醇水溶液進行吸附與100 %乙醇進行脫附後，黃酮類含量提高至25.9%，內酯類含量提高至7.3 %，兩類的濃縮比均約為5倍，而均有極高的回收率(大於99 %)，另外，目前總提取濃縮比例約為34：1，容許我們可藉階段脫附之操作再進一步提高兩類的含量，但以此系統而言，階段脫附所造成之提高效果並不明顯。

The Ginkgo biloba dried leaves imported from China were used as the starting material. First, this study investigated the leaching efficiency of the Soxhlet extractor using ethanol as the leaching solvent, the optimal leaching conditions were determined by experimental design and regression analysis. Then, the extracted product was further isolated and purified in preparative-scale by the adsorptive liquid chromatography technology. The results show that the concentrations of flavonoids and terpenes in the extracted product were 2.5 % and 0.3 % respectively, using the best leaching conditions: 160 ml, 70 % ethanol solution and 3 hrs. Their concentrations were then raised to be 4.9 % and 1.3 % respectively after being dissolved by the 10 % ethanol solution. Finally, their concentrations were raised to be 25.9 % and 7.3 % respectively after being isolated by the XAD7 resin column (10 % and 100 % ethanol solution for the adsorption and desorption step, respectively). The concentration factors were about 5 and the recoveries were greater than 99 % for both flavonoids and terpenes. The overall leaching ratio from the dried leaves was about 38:1, which allows us to further concentrate both contents by using the step-wise elution method, but for current system the effect of the step-wise elution method was not significant .

目錄
中文摘要 ··········································································································· i
英文摘要 ··········································································································· ii
誌謝 ··········································································································· iii
目錄 ··········································································································· iv
表目錄 ··········································································································· vi
圖目錄 ··········································································································· vii
一、 緒論···································································································· 1
二、 文獻回顧與理論部分········································································ 3
2.1 銀杏的有效成分················································································ 3
2.2 銀杏成分的藥理作用········································································ 3
2.3 銀杏中之有毒成分············································································ 3
2.4 銀杏萃取物製備方法的文獻回顧···················································· 11
2.5 銀杏有效成分分析方法的文獻回顧················································ 11
2.6 XAD微孔介質的介紹······································································· 11
2.7 實驗設計理論···················································································· 17
2.8 固相萃取法(solid phase extraction , or SPE)的層析理論··············· 20
2.9 放大設計與操作理論········································································ 24
三、 材料與方法························································································ 28
3.1 實驗材料與儀器················································································ 28
3.2 實驗步驟···························································································· 31
3.2.1 銀杏葉提取步驟················································································ 31
3.2.1.1 以索氏提取法進行銀杏葉之提取···················································· 31
3.2.2 HPLC分析························································································· 31
3.2.2.1 黃酮類之HPLC定量分析································································ 31
3.2.2.2 內酯類之HPLC定量分析································································ 33
3.2.3 粗提液的進一步濃縮純化································································ 37
3.2.3.1 粗提液轉溶為原液之損失以及偵測原液溶解度之實驗步驟········ 37
3.2.3.2 管柱層析分離法················································································ 38
四、 結果與討論························································································ 41
4.1 銀杏葉溶劑提取物的HPLC分析···················································· 41
4.1.1 最佳黃酮糖甘水解條件之決定與黃酮類之HPLC分析················· 41
4.1.2 內酯類之HPLC分析········································································ 48
4.2 最佳銀杏葉溶劑提取條件的選取···················································· 52
4.2.1 索氏提取黃酮類的實驗結果、統計分析及最佳操作條件的
找尋···································································································· 52
4.3 偵測粗提液轉溶為原液之損失以及原液溶解度之實驗量測········ 59
4.3.1 轉溶損失的量測················································································ 59
4.3.2 原液中黃酮類與內酯類溶解度的量測············································ 59
4.4 管柱層析分離法的濃縮純化效果···················································· 59
4.4.1 動態吸附與脫附實驗以及濃縮與純化效果的計算························ 59
4.4.2 脫附液組成與脫附時間對濃縮純化效果的影響···························· 66
4.4.3 提高原液濃度對純化效果的影響···················································· 72
4.4.4 進一步提高濃縮比之方法································································ 75
4.5 XAD-7管柱的放大設計與操作······················································· 78
五、 結論···································································································· 80
六、 參考文獻···························································································· 81
附錄A 黃酮類對內酯類分析之影響···························································· 84
附錄B 使用雙柱法與直接分析法分析內酯類之結果比較以及雙柱
法內部流程之內酯類損失································································ 88
附錄C 內酯類對黃酮類分析之影響···························································· 93
附錄D 孔隙度的量測與分析方法································································ 97

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