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研究生:周詩音
研究生(外文):CHIEW SOO IM
論文名稱:正交試驗法優化芳香萬壽菊葉精油萃取之研究
論文名稱(外文):Optimization of Essential Oil Extraction for Tagetes Lemmonii Leaves Using Orthogonal Array Design
指導教授:蔡鳳婕
指導教授(外文):TSAI, FENG-JIE
口試委員:李茂榮李名鏞
口試委員(外文):LEE, MAW-RONGLEE, MING-TUNG
口試日期:2016-06-20
學位類別:碩士
校院名稱:靜宜大學
系所名稱:化粧品科學系
學門:民生學門
學類:美容學類
論文種類:學術論文
論文出版年:2016
畢業學年度:104
語文別:中文
論文頁數:121
中文關鍵詞:芳香萬壽菊正交實驗設計精油原精頂空-固相微萃取
外文關鍵詞:Tagetes LemmoniiOrthogonal Array Experimental DesignEssential oilConcreteHeadspace - solid phase micro extraction
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本研究利用 正交實驗設計結合統計分析方法,探討經由傳統之水蒸餾和水蒸氣蒸餾之綠色萃取方法,萃取在不同之季節新鮮與乾燥芳香萬壽菊(Tagetes Lemonnii)葉,探討其精油的量及DPPH自由基清除能力之變化,分別依精油含量, DPPH自由基清除率及總清除DPPH能力為指標,由直觀分析和變異數分析 (Analysis of variance, Anova) 得最適化之萃取條件及變因影響之關係。比較以優條件萃取所得之精油與原精、頂空-固相微萃取(Head space-solid phase microextraction, HS-SPME)方法,所得之其成分差異,及以Flavornet輔助判別氣味差異。
研究結果得知,芳香萬壽菊秋季與春季之優化萃取條件相同,以水蒸餾萃取法,萃取新鮮植物,萃取時間為4 hrs,無需浸泡,料液比為1:15 。秋季之精油萃取率為0.102 % - 0.394 %;冬春季為0.091 % - 0.233 %。從精油量T-檢定結果得知,春季與秋季精油量有顯著差異。經Anova分析,以精油量及DPPH抗氧化能力為指標的因子並無明顯差異。不同萃取方法的精油經鑑定,秋季有30種化合物;春季有26種化合物。其中精油主成分為Cis-β-Ocimene、Dihydrotagetone 、Trans-β-Ocimene、Artemisia ketone、Trans-Epoxyocimene、Cis-Tagetone、Trans-Tagetone、 phenol, m-tert-butyl-、Levoverbenone、Germacrene D。而以HS-SPME於高溫萃取,則比精油成分少Cis-β-Ocimene及Artemisia ketone ;HS-SPME於室溫 萃取則少Cis-Tagetone成分;在溶劑萃取下,則少Cis-β-Ocimene、Artemisia ketone、Phenol, m-tert-butyl-。綜合以上相同主成分含有之氣味為:floral-fruity, tagete, citrus fruit, chemical, deodorant, floral, minty, plastic, vegetable, geranium, woody and spice。
An investigation was focus on the difference between seasons and dry/fresh plant to find out the optimum condition of Tagetes Lemmonnii leaves. Different green traditional extraction method such as Water Distillation, Steam Distillation have been performed using Orthogonal Array Design and statistical analysis. In addition, optimum extraction conditions will available due to the influence of factors, at the same time, content, capacity of DPPH radical scavenging and total clearance of DPPH of the essential oil(EO) would be as an assessment criteria by visual analysis and variance analysis (ANOVA). Moreover, used hexane as the solvent of concrete extraction and headspace - solid phase micro extraction (HS-SPME) of volatile organic compounds extraction, analyses, then compare their components and auxiliary discriminating flavour difference by using Flavornet.
As a result of the experiment, using the water distillation extraction method, fresh plant without soaking, 1: 15 ratio for plant and liquid, and 4 hrs extraction was found as the same of optimal extraction condition in Autumn’s plant and Sping’s plant. The range percentage of essential oil for Autumn’s plant was 0.102%-0.394%, the range of essential oil for Spring’s plant was 0.091%-0.233%. From the results that amount of essential oil,Spring’s oil is less than Autumn’s oil. The T-test result showed that no differ significant between Spring’s oil and Autumn’s oil. DPPH antioxidant capacity were not significantly different (p>0.05). In total, 30 and 26 compounds were identified in the Autumn’sEO and Spring’s EO respectively. The main component such as Cis-β-Ocimene, Dihydrotagetone, Trans-β-Ocimene, Artemisia ketone, Trans-Epoxyocimene, Cis-Tagetone, Trans-Tagetone, phenol, m-tert-butyl-, Levoverbenone, Germacrene D being the most abundant constituents in essential oil. At the high room temperature SPME extraction have the similar component with EO except Cis-β-Ocimene and Artemisia ketone. Under the room temperature SPME extraction the component almost same with EO except Cis-Tagetone. Besides that, Cis-β-Ocimene、Artemisia ketone、Phenol, m-tert-butyl- were not found in concrete which extract by solvent The Main flavor such as citrus, herb, flower, floral-fruity, tagete, citrus fruit, chemical, deodorant, floral, minty, plastic, vegetable, geranium, woody and spice were identified.
謝誌 I
摘要 II
Abstract IV
Abbreviation VI
目錄 VIII
圖目錄 XI
表目錄 XIII
壹、前言 1
1.1 芳香萬壽菊Tagetes Lemmonii簡介 4
1.2 植物精油及揮發性化合物萃取方法 11
1.2.1 水蒸餾與水蒸氣蒸餾法 (WD and SD) 17
1.2.2 溶劑萃取法(SE) 18
1.2.3 頂空-固相微萃取法(HS-SPME) 19
1.3 抗氧化性之效能估 23
1.4 正交實驗設計法與統計分析 29
1.4.1 正交實驗設計(Orthogonal Array experimental design) 29
1.4.2 直觀分析法(Intiutive analysis method) 34
1.4.3 變異數分析(Analysis of variance, ANOVA) 36
1.5 定性—精油及揮發物之分析 39
1.6 定量—面積歸一化法分析 45
1.7 氣味鑑定 46
1.8 研究目的 47
貳、 實驗 48
2.1 材料與試劑 48
2.2 儀器與萃取裝置設備 50
2.3 實驗架構及實驗方法 52
2.3.1 精油萃取之實驗參數及水平設定 53
2.4 精油萃取步驟 55
2.4.1 水蒸餾萃取法 55
2.4.2 蒸氣蒸餾萃取法 55
2.4.3 頂空-固相微萃取(HS-SPME)法 57
2.4.3.1 HS-SPME室溫萃取 57
2.4.3.2 HS-SPME高溫萃取 57
2.4.4 溶劑萃取法59
2.5 清除DPPH自由基之抗氧化能力測定 60
2.6 數據統計與分析 62
參、結果與討論 63
3.1 不同季節之芳香萬壽菊精油萃取之優化條件探討 63
3.1.1 秋季植物萃取之直觀分析與變異數分析結果 65
3.1.2 春季植物萃取之直觀分析與變異數分析結果 73
3.1.3 不同季節植物精油比較 79
3.2 精油成份定性與氣味鑑定結果 82
3.3 精油萃取、溶劑萃取、頂空固相微萃取之比較 93
3.3.1 頂空-固相微萃取成份及氣味結果 93
3.3.2 精油萃取與頂空-固相微萃取成份及氣味之比較 99
3.3.3 精油萃取與溶劑萃取成份及氣味之比較 104
肆、結論 108
伍、未來展望 111
陸、文獻參考 112
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