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研究生:陳怡婷
研究生(外文):Yi-Ting Chen
論文名稱:雷射脫附離子化質譜術分析小分子和超臨界流體萃取抗阿爾茲海默氏症藥用植物之研究
論文名稱(外文):Analysis of Low-Molecular Weight Compounds by Laser desorption/Ionization Mass Spectrometry & Supercritical Fluid Extraction and Preparation of Effective Ingredients of L. serratum and Ginkgo for Treating Alzheimer''s Diasease.
指導教授:凌永健凌永健引用關係
指導教授(外文):Yong-Chien Ling
學位類別:博士
校院名稱:國立清華大學
系所名稱:化學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:中文
論文頁數:300
中文關鍵詞:雷射脫附離子化質譜術基質輔助雷射脫附離子化質譜術紫質苯二甲藍素阿爾茲海默氏症超臨界流體萃取銀杏內酯長柄千層塔石杉鹼甲
外文關鍵詞:LDlaser desorption ionization mass spectrometryMALDImatrix-assisted laser desorption ionozation mass spectrometryporphyrinPhthalocyanineAlzheimer''''s diseaseSupercritical Fluid ExtractionGinkgolidehuperzine A
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新技術的快速發展,及人類追求生活水準的提升,因此製造出五花八門的生活用品,例如食品、藥物及資訊產業等相關產品。產品研發過程中,需要適當的分析儀器與分析方法,持續研發、調整生產製程,以獲取最佳產品品質。質譜術新型游離法的發展,在生化及工業高分子的應用助益頗大。本論文發展(基質輔助)雷射脫附離子化質譜術於小分子的分析應用,及建立抗阿爾茲海默氏症藥用植物之綠色製程超臨界流體萃取技術。本論文共分為五章:
一、緒論
二、發展紫質基質輔助雷射脫附離子化飛行時間質譜術定量分析水溶性維他命
三、單寫式光碟片用染料─苯二甲藍素之脫附質譜研究
四、超臨界流體萃取銀杏葉中之銀杏內酯類化合物之研究
五、超臨界流體萃取長柄千層塔中之石杉鹼甲之研究
第一部份「雷射脫附離子化質譜術分析小分子之研究」涵蓋第二章及第三章,第二章使用基質輔助雷射脫附離子化質譜術分析水溶性維他命,首次探討17種紫質基質的適用性,建立快速半定量分析水溶性維他命之方法;第三章建立以雷射脫附離子化質譜術及基質輔助雷射脫附離子化質譜術監測光碟片染料¾苯二甲藍素之新分析方法,並應用至合成反應的監測,由質譜結果獲得較可見光光譜更為精確的結構資訊及產物分子的生成比例;第二部分「超臨界流體萃取抗阿爾茲海默氏症藥用植物之研究」涵蓋第四章及第五章,第四章以田口式實驗計畫法決定超臨界流體萃取銀杏內酯A及B之實驗參數最佳化組合,以修飾劑量為顯著因子,初步測試市售銀杏萃取物商品;第五章首次以超臨界流體萃取石杉鹼甲,並以田口式實驗計畫法決定超臨界流體萃取實驗參數之最佳化組合。
目 錄
頁次
第1章 緒論……………….…………………………………………...1-1
1.1 前言.……………………………………………………………….1-1 1.2 研究動機與目的1-1
1.2.1 雷射脫附離子化質譜術分析小分子之應用1-1
1.2.2 超臨界流體萃取抗阿爾茲海默氏症藥用植物之研究1-2
1.3 參考文獻1-3
第2章 發展紫質基質輔助雷射脫附離子化飛行時間質譜術定量分析水溶性維他命2-1
2.1 前言……………………….……...…………………….….2-1
2.1.1 基質輔助雷射脫附離子化飛行時間質譜術2-2
2.2 研究動機2-12
2.2.1 紫質之簡介2-14
2.2.2 紫質於基質輔助雷射脫附離子化質譜之應用2-14
2.3 實驗部份2-16
2.3.1 儀器設備2-16
2.3.2 藥品來源2-17
2.3.3 基質輔助雷射脫附離子化質譜術標準品製備方法2-19
2.4 結果與討論2-20
2.4.1 依有效質譜視窗選擇基質2-20
2.4.2 基質/待測物莫耳比對基質輔助雷射脫附效應之影響2-21
2.4.3 紫質基質結構對基質輔助雷射脫附效應之影響2-23
2.4.4 定量內標的選擇2-24
2.4.5 定量分析2-26
2.4.6 真實樣品之製備及分析2-29
2.5 結論2-31
2.6 參考文獻2-32
第3章 單寫式光碟片用染料─苯二甲藍素之脫附質譜研究……..3-1
3.1 前言………………………………………………………………..3-1 3.1.1 原理3-2
3.1.2 市場3-2
3.1.3 技術及染料3-4
3.2 研究動機及目的3-6
3.2.1 苯二甲藍素之性質3-6
3.2.2 苯二甲藍素之雷射脫附質譜分析3-7
3.3 實驗部分3-8
3.3.1 試藥3-8
3.3.2 儀器設備3-9
3.3.3 合成與分析方法3-10
3.4 結果與討論3-18
3.4.1 解析度之探討3-18
3.4.2 脫附離子質譜圖特性離子3-18
3.4.3 NiPC之合成與分析3-20
3.4.4 CuPC之合成與分析3-23
3.5 結論與展望3-24
3.6 參考文獻……………..…………………………………………..3-26
第4章 超臨界流體萃取銀杏葉中之銀杏內酯類化合物之研究……4-1
4.1 前言………………………………………………………..4-1
4.1.1 失智症簡介4-2
4.1.2 健康食品及中草藥4-9
4.2 研究動機4-15
4.3 研究方法4-16
4.3.1 銀杏4-16
4.3.2 超臨界流體萃取4-19
4.3.3 實驗計畫法4-24
4.3.4 銀杏樣品及分析方法4-26
4.4 材料、儀器設備及實驗方法4-28
4.4.1 試藥4-28
4.4.2 藥材及樣品4-29
4.4.3 儀器設備4-29
4.4.4 實驗方法4-30
4.5 結果與討論4-38
4.5.1 分析方法4-38
4.5.2 衍生反應條件4-39
4.5.3 銀杏水萃液添加方式4-39
4.5.4 田口式實驗計畫法4-40
4.5.5 真實樣品分析4-44
4.6 結論4-47
4.7 參考文獻4-48
第5章 超臨界流體萃取長柄千層塔中之石杉鹼甲之研究5-1
5.1 前言…………………………………………………………..5-1
5.1.1 石杉鹼甲5-1
5.2 研究動機5-4
5.3 材料與實驗方法5-5
5.3.1 試藥5-5
5.3.2 藥材及樣品5-6
5.3.3 實驗設備5-6
5.3.4 實驗方法5-7
5.4 結果與討論5-11
5.4.1 HPLC-UV檢量線建立5-11
5.4.2 添加方式評估5-11
5.4.3 田口式實驗計畫法5-12
5.4.4 回收率與再現性5-15
5.5 結論5-16
5.6 參考文獻5-17
表 目 錄
頁次
第2章 發展紫質基質輔助雷射脫附離子化飛行時間質譜術定量分析水溶性維他命
表2-1常見的基質結構、配置方法及適用待測物…………………...2-43
表2-2紫質、內標及維他命的化學結構、分子式、分子量及溶劑…...2-47
表2-3紫質、內標及內標準品之LD-TOFMS特性離子峰…………2-52
表2-4紫質於雷射脫附離子化質譜圖之雷射能量及背景干擾比較表……………………………………………………………….2-57
表2-5各維他命於MALDI-TOFMS之特性離子峰、最適化M/A值及定量用基質………………………………………………….2-58
表2-6維他命及紫質之lmax及l………………………………………2-59
表2-7再現性評估…………………………………………………….2-60
表2-8維他命B1、B2、B6、B12及C之檢量線比較表…………………..2-61
表2-9各維他命於各濃度之RSD、及計算出之LOD及LOQ……….2-62
表2-10市售單一及複合維他命樣品之MALDI-TOFMS分析結果…2-63
第3章 單寫式光碟片用染料─苯二甲藍素之脫附質譜研究
表3-1CD系統規格…………………………………………………...3-29
表3-2CD-R光碟片台灣與日本產量消長變化……………………...3-30
表3-3台灣CD-R光碟片材料及化學品市場需求…………………...3-30
表3-4三種主要CD-R光碟片用染料之比較………………………...3-31
表3-5NiPC之LD-TOFMS特性離子………………………………...3-32
表3-6NiPCBrx之LD-TOFMS特性離子……………………………..3-33
表3-7CuPC之LD-TOFMS特性離子………………………………..3-34
表3-8CuPCBrx之LD-TOFMS特性離子……………………….……3-35
表3-9NiPC之MALDI-TOFM'S特性離子…………………………..3-36
表3-10NiPCBrx之MALDI-TOFMS特性離子………………………..3-37
表3-11CuPC之MALDI-TOFMS特性離子…………………………..3-38
表3-12CuPCBrx之MALDI-TOFMS特性離子……………………….3-39
表3-13NiPCBrx溴化反應之最大吸收波長…………………………...3-40
表3-14CuPCBrx溴化反應之最大吸收波長……………….………….3-40
第4章 超臨界流體萃取銀杏葉中之銀杏內酯類化合物之研究
表4-1失智症的三大類症狀………………………………………….4-60
表4-2臺灣地區老年失智人口的推估……………………………….4-60
表4-3阿爾茲海默氏症患者個人及整體社會預估所需支出費用…4-61
表4-4阿爾茲海默氏症乙醯膽鹼酵素抑制劑之臨床試驗及其作用機轉…………………………………………………………….4-62
表4-51997年世界中草藥補品市場統計表………………………….4-63
表4-61997年歐洲中草藥膳食補充品的銷售額…………………….4-63
表4-71997年美國中草藥膳食補充品的功效及銷售額銷售額…….4-64
表4-81999年美國中草藥膳食補充品的相對銷售比例…………….4-66
表4-9具有潛力之抗阿爾茲海默氏症藥用植物及其有效成分…….4-67
表4-10銀杏濃縮物藥物動力學資料………………………………….4-68
表4-11銀杏葉萃取物的組成………………………………………….4-68
表4-12歐洲允許GMP製程使用之萃取溶劑………………………...4-69
表4-13歐洲對於食品工業萃取溶劑之使用狀況及殘留量之規範….4-69
表4-14歐洲對於食品工業萃取溶劑之使用狀況及殘留量之規範….4-70
表4-15美國使用於食品之部分溶劑用途及其殘留標準…………….4-71
表4-16我國溶劑類食品添加物使用範圍及用量標準……………….4-72
表4-17二氧化碳的氣體、液體和超臨界流體物理性質之比較……...4-73
表4-18適合作為壓縮溶劑之氣體及其性質………………………….4-73
表4-19超臨界流體萃取之代表性天然物…………………………….4-74
表4-20超臨界流體萃取植物中有效成分與傳統方法之比較……….4-75
表4-21銀杏內酯A及B衍生物之MS及MS-MS特性離子列表…….4-76
表4-22銀杏內酯添加方式比較表…………………………………….4-76
表4-23田口式實驗計畫法於超臨界流體萃取銀杏內酯A及B之實驗條件配置…………………………………………………….4-77
表4-24超臨界流體萃取中藥銀杏葉之有效成份¾銀杏內酯A及B各因子變數水準表…………………………………………….4-77
表4-25超臨界流體萃取銀杏內酯A之變異數分析表……………….4-78
表4-26超臨界流體萃取銀杏內酯B之變異數分析表……………….4-78
表4-27超臨界流體萃取銀杏內酯A各因子於各水準之水準效果值.4-79
表4-28超臨界流體萃取銀杏內酯B各因子於各水準之水準效果值.4-79
表4-29萃取方法代號表……………………………………………….4-79
表4-30真實樣品……………………………………………………….4-80
表4-31超臨界流體萃取市售樣品之銀杏內酯A含量……………….4-81
表4-32超臨界流體萃取市售樣品之銀杏內酯B含量……………….4-82
第5章 超臨界流體萃取長柄千層塔中之石杉鹼甲之研究………….…..5-1
表5-1田口式實驗計畫法於超臨界流體萃取石杉鹼甲之實驗條件配置…………………………………………………………….5-21
表5-2超臨界流體萃取中藥長柄千層塔之有效成份¾石杉鹼甲各因子變數水準表……………………………………………….5-21
表5-3超臨界流體萃取石杉鹼甲之變異數分析表………………….5-22
表5-4超臨界流體萃取石杉鹼甲各因子於各水準之水準效果值5-22
圖 目 錄
頁次
第2章 發展紫質基質輔助雷射脫附離子化飛行時間質譜術定量分析水溶性維他命
圖2-1直線型飛行時間質譜儀示意圖……………………………..2-64
圖2-2反射型飛行時間質譜儀示意圖……………………………..2-64
圖2-3雙階程反射型飛行時間質譜儀…………………………….2-65
圖2-4同軸反射型反射型飛行時間質譜儀………………………..2-65
圖2-5延遲汲取示意圖……………………………………………..2-66
圖2-6延遲汲取及連續汲取操作比較圖示意圖…………………...2-66
圖2-7基質輔助雷射脫附離子化質譜數樣品置備/分析流程圖…..2-67
圖2-8基質輔助雷射脫附離子化示意圖…………………………...2-67
圖2-9紫外光基質輔助雷射脫附光化學離子化途徑………….…..2-68
圖2-10有機小分子的光化學離子化途徑…………………………...2-68
圖2-11吡咯及紫質的基本結構……………………………………...2-69
圖2-12Sinapinic acid之低能量雷射脫附正離子質譜圖………..…..2-70
圖2-13Sinapinic acid之高能量雷射脫附離子化質譜圖…………....2-70
圖2-14紫質PP之雷射脫附正離子質譜圖…………………………2-71
圖2-15紫質PP之雷射脫附負離子質譜………………………….…2-71
圖2-16紫質CP之雷射脫附正離子質譜圖…………………………2-72
圖2-17紫質CP之雷射脫附負離子質譜圖…………………………2-72
圖2-18紫質PTTB之雷射脫附正離子質譜圖……………………....2-73
圖2-19紫質PTTB之雷射脫附負離子質譜圖……………………...2-73
圖2-20紫質TMPP之雷射脫附正離子質譜圖……………………....2-74
圖2-21紫質TMPP之雷射脫附負離子質譜圖………………………2-74
圖2-22紫質TPDP之雷射脫附正離子質譜圖………………………2-75
圖2-23紫質TPDP之雷射脫附負離子質譜圖………………………2-75
圖2-24紫質THPP之雷射脫附正離子質譜圖………………………2-76
圖2-25紫質THPP之雷射脫附負離子質譜圖……..………………..2-76
圖2-26紫質MP之雷射脫附正離子質譜圖…………………………2-77
圖2-27紫質MP之雷射脫附負離子質譜圖…………………………2-77
圖2-28紫質TDCPP之雷射脫附正離子質譜圖………………..……2-78
圖2-29紫質TDCPP之雷射脫附負離子質譜圖……………………..2-78
圖2-30紫質TTMPPP之雷射脫附正離子質譜圖…………………...2-79
圖2-31紫質TTMPPP之雷射脫附負離子質譜圖…………………...2-79
圖2-32紫質TCMPP之雷射脫附正離子質譜圖……………………2-80
圖2-33紫質TCMPP之雷射脫附負離子質譜圖……………………2-80
圖2-34紫質EP之雷射脫附正離子質譜圖..………………………...2-81
圖2-35紫質EP之雷射脫附負離子質譜圖..………………………...2-81
圖2-36紫質OEP之雷射脫附正離子質譜圖………………………..2-82
圖2-37紫質OEP之雷射脫附負離子質譜圖………………………..2-82
圖2-38紫質OBNC之雷射脫附正離子質譜圖..…………………….2-83
圖2-39紫質OBNC之雷射脫附負離子質譜圖..……………………2-83
圖2-40紫質TCPPC之雷射脫附正離子質譜圖……………………2-84
圖2-41紫質TCPPC之雷射脫附負離子質譜圖……………………..2-84
圖2-42紫質TPFPP之雷射脫附正離子質譜圖……………………...2-85
圖2-43紫質TPFPP之雷射脫附負離子質譜圖……………………...2-85
圖2-44紫質TMAP之雷射脫附正離子質譜圖……………………...2-86
圖2-45紫質TMAP之雷射脫附負離子質譜圖……………………...2-86
圖2-46紫質TPP之雷射脫附正離子質譜圖………………………...2-87
圖2-47紫質TPP之雷射脫附負離子質譜圖………………………...2-87
圖2-48紫質PTTB與維他命B12之不同M/A值之正離子基質輔助雷射脫附質譜圖……………………………………………...2-88
圖2-49紫質PTTB與維他命C之不同M/A值之負離子基質輔助雷射脫附質譜圖……………………………...………………2-88
圖2-50紫質THPP與維他命C之不同M/A值之負離子基質輔助雷射脫附質譜圖……………...………………………………2-89
圖2-51紫質PTTB與維他命B1之不同M/A值之正離子基質輔助雷射脫附質譜圖………………………………...……………2-89
圖2-52紫質THPP與維他命B2之不同M/A值之基質輔助雷射脫附質譜圖…………………..………………………………….2-90
圖2-53紫質PTTB與維他命B6之不同M/A值之正離子基質輔助雷射脫附質譜圖……………………………………………...2-90
圖2-54維他命B1、C及B6於不同紫質基質下之訊/雜比…………...2-91
圖2-55維他命B1特性離子[M-Cl]+強度隨著雷射脈衝數目增加的變化…………………………………………………………...2-91
圖2-56結晶之光學顯微鏡結果……………………………………...2-92
第3章 單寫式光碟片用染料─苯二甲藍素之脫附質譜研究
圖3-1CD-R之構造……...………………….……………………….3-41
圖3-2我國光碟片市場概況……………………...…………………3-41
圖3-3光碟片成本結構圖….……………………..…………………3-42
圖3-4花青素的基本結構…………………………...………………3-42
圖3-5苯二甲藍素的基本結構………………………...……………3-43
圖3-6CuPC合環反應稀釋及淨化步驟……………………….……3-43
圖3-7不同儀器參數所得之高中低解析度比較圖………………...3-44
圖3-8all-trans Retinoic acid基質之雷射脫附離子化質譜圖……..3-44
圖3-9NiPC及NiPCBrx之低解析LD及MALDI-TOFMS質譜圖…3-45
圖3-10NiPC及NiPCBrx之高解析LD及MALDI-TOFMS質譜圖…3-45
圖3-11CuPC及CuPCBrx之低解析LD及MALDI-TOFMS質譜圖..3-46
圖3-12CuPC及CuPCBrx之高解析LD及MALDI-TOFMS質譜圖..3-46
圖3-13(a)3-Nitrophthalonitrile接側鏈反應之反應機制;(b)NiPC合環反應之反應機制………………………………………...3-47
圖3-14NiPCBrx溴化反應之反應機制………………………………3-47
圖3-15低解析雷射脫附離子化質譜監測NiPC合環反應之系列質譜圖…………………………………………………………...3-48
圖3-16低解析雷射脫附離子化質譜監測NiPCBrx溴化反應之系列質譜圖………………………………………………………...3-48
圖3-17高解析雷射脫附離子化質譜監測NiPC合環反應之系列質譜圖…………………………………………………………...3-49
圖3-18高解析雷射脫附離子化質譜監測NiPCBrx溴化反應之系列質譜圖………………………………………………………...3-49
圖3-19NiPCBr(994.8 Da)之離子源後續衰變圖…………………...3-50
圖3-20低解析基質輔助雷射脫附離子化質譜術監測NiPC合環反應之系列質譜圖……………………………………………...3-50
圖3-21低解析基質輔助雷射脫附離子化質譜術監測NiPCBrx溴化反應之系列質譜圖…………………………………………...3-51
圖3-22高解析基質輔助雷射脫附離子化質譜術監測NiPC合環反應之系列質譜圖……………………………………………...3-51
圖3-23(a)高解析基質輔助雷射脫附離子化質譜術監測NiPCBrx溴化反應之系列質譜圖……………………………………...3-52
圖3-23(b)圖3-23(a)之局部放大圖……………………………….3-52
圖3-24NiPCBrx溴化分子(x=1~6)面積比對反應時間做圖………..3-53
圖3-25NiPCBrx溴化反應之可見光吸收光譜反應監測……………3-53
圖3-26高解析雷射脫附離子化質譜監測CuPC合環反應之系列質譜圖…………………………………………………………...3-54
圖3-27 高解析雷射脫附離子化質譜監測CuPCBrx溴化反應之系列質譜圖……………………………………………………...3-54
圖3-28 高解析基質輔助雷射脫附離子化質譜監測CuPC合環反應之系列質譜圖………………………………………………...3-55
圖3-29高解析基質輔助雷射脫附離子化質譜監測CuPCBrx溴化反應之系列質譜圖…………………………………………...3-55
圖3-30 CuPCBrx溴化反應之可見光吸收光譜反應監測……………3-56
第4章 超臨界流體萃取銀杏葉中之銀杏內酯類化合物之研究
圖4-1台灣65歲以上老人人口佔總人口比重統計表……………..4-83
圖4-2銀杏之照片…………………………………………………...4-83
圖4-3銀杏葉萃取物中類黃酮化合物結構之化學結構圖………...4-84
圖4-4銀杏葉萃取物中帖烯內酯化合物結構之化學結構圖……...4-85
圖4-5二氧化碳之三相圖及等密度線……………………………...4-86
圖4-6SFE應用於萃取植物有益成分及有害成分之文獻發表統計圖……………………………………………………………...4-86
圖4-7典型銀杏內酯之液液萃取、純化步驟……………………….4-87
圖4-8實驗所用超臨界流體裝置示意圖…………………………...4-88
圖4-9銀杏內酯A及B液液萃取、超臨界流體萃取流程圖……….4-89
圖4-10銀杏葉真實樣品超臨界流體萃取槽填充方式……………...4-90
圖4-11銀杏內酯A之GC-FID檢量線……………………………….4-90
圖4-12銀杏內酯B之GC-FID檢量線……………………………….4-91
圖4-13角鯊烷、銀杏內酯A及B標準品衍生產物之氣相層析四極柱質譜儀選擇離子掃描層析圖…………………………...4-91
圖4-14(a)、角鯊烷、銀杏內酯A及B標準品衍生物之氣相層析離子阱質譜儀總離子層析圖………………………………...4-92
圖4-14(b)、銀杏內酯A標準品衍生產物之氣相層析離子阱質譜儀全離子掃描質譜圖………………………………………...4-92
圖4-15(a)、銀杏內酯A及B標準品衍生物之氣相層析離子阱質譜儀串連質譜離子層析圖…………………………………...4-93
圖4-15(b)、銀杏內酯A標準品衍生產物之537 Da離子之氣相層析離子阱質譜儀串連質譜圖……………………………...4-93
圖4-16銀杏內酯B標準品衍生產物之氣相層析離子阱質譜儀全離子掃描質譜圖……………………………………………...4-94
圖4-17銀杏內酯B標準品衍生產物之625 Da離子之氣相層析離子阱質譜儀串連質譜圖……………………………………...4-94
圖4-18(a)、銀杏真實樣品之超臨界流體萃取氣相層析四極柱質譜儀總離子層析圖…………………………………………...4-95
圖4-18(b)、超臨界流體萃取銀杏真實樣品,衍生後之選擇離子掃描層析圖…………………………………………………...4-95
圖4-19超臨界流體萃取實驗計畫法結果之最適化條件GC-FID分析結果………………………………………………………...4-96
圖4-20超臨界流體系統空白之GC-FID分析結果………………….4-96
圖4-21超臨界流體可使用之收集裝置示意圖……………………...4-97
圖4-22超臨界流體萃取銀杏內酯A各因子於各水準之水準效果值……………………………………………………………...4-98
圖4-23超臨界流體萃取銀杏內酯B各因子於各水準之水準效果值……………………………………………………………...4-99
圖4-24真實樣品之照片……………………………………………...4-100
圖4-25市售銀杏樣品之分析結果作圖……………………………...4-104
圖4-26市售銀杏樣品C之超臨界流體直接萃取藥錠GC-FID結果.4-104
第5章 超臨界流體萃取長柄千層塔中之石杉鹼甲之研究…...…………5-1
圖5-1石杉鹼甲之化學結構………………………………………...5-23
圖5-2長柄千層塔之外觀…………………………………………...5-23
圖5-3消旋石杉鹼甲合成途徑之一………………………………...5-24
圖5-4液液萃取製備石杉鹼甲標準品流程圖……………………...5-25
圖5-5石杉鹼甲之紫外光吸收光譜圖……………………………...5-26
圖5-6市售石杉鹼甲標準品及定量內標準品之液相層析圖譜…...5-26
圖5-7石杉鹼甲之檢量線(1.0-25.0 ppm)…………………………..5-27
圖5-8自行置備之石杉鹼甲溶液液相層析圖譜…………………...5-27
圖5-9超臨界流體萃取石杉鹼甲實驗計畫法結果之液相層析分析結果之一…………………………………………………...5-28
圖5-10系統空白之液相層析分析結果……………………………...5-28
圖5-11超臨界流體萃取石杉鹼甲各因子於各水準之水準效果值...5-29
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