臺灣博碩士論文加值系統

長久以來，護膚產品的添加物已經開始改變。因為空氣污染、室內空調、臭氧層的破洞、紫外線的照射和緊張、快步調的生活模式，皆會造成皮膚的損傷與不健康，皮膚護理產品需要對這些變化作出回應，近年來，化妝品界發現金合歡醇是不錯的皮膚護理成分。
本研究是建立一套GC分析方法來檢測美容水膠貼布中金合歡醇的成分的含量與穩定性，管柱是Varian 公司 VA-1型號，載流氣體為氮氣，注射口溫度：250 ℃，火焰離子化偵測器溫度：280 ℃，分流比：50：1，流速：12.66 psi，注射量：1 μL，烘箱溫度變化起始溫度為80 ℃，每分鐘上升10 ℃至130 ℃，接著再以每分鐘100 ℃上升至260 ℃後維持3.5分鐘，此分析方法可以在10分鐘內完成。
在分析確效方面，金合歡醇的線性迴歸係數為R2 ＝ 0.9997，精密度實驗的相對標準偏差( RSD) 介於0.7970 ％到1.6691 ％之間，準確度實驗的回收率則介於95.1 ％至104.2 ％之間，偵測極限和定量極限分別為2 ppm以及7 ppm。
在安定性試驗方面，美容水膠貼布的主成分金合歡醇分別在(25 ± 2 ℃)及(40 ± 2 ℃)的環境下進行實驗，經過6個月後發現外觀皆無明顯的變化，但金合歡醇的含量分別降至92.78 ％及88.01 ％。

Recently, the additive of skin care products has been gradually changed. Since Air pollution, overusing air-conditioner, ozone hole, ultraviolet radiation and tense, fast-paced lifestyle have caused the skin damage and unhealthy. The content of skin care products need to change to respond the environmental variation. Lately, cosmetic scientist found that farnesol is a relatively good ingredient in skin health.
In the research, a gas chromatography method was developed to determine the content and stability of farnesol in beauty hydrogel patch. The VA-1 type column made by Varian company is using and carrier gas is nitrogen. The injection temperature: 250 ℃, FID detection temperature: 280 ℃, split: 1: 50, flow rate at a linear velocity of 12.66 psi, an injection volume: 1 μL. The oven temperature was programmed from 80 ℃ held for 0 min , then 10 ℃/min ramp to 130 ℃, then 100 ℃/min ramp to 260 ℃ held for 3.5 min. Total run time was 10 min.
In the analytical method validation of farnesol in beauty hydrogel patch, the results of relative standard deviation are between 0.797 % and 1.6691 %; the results of recovery are between 95.1 % and 104.2 %; the result of linear regression coefficient is 0.9997; the result of limit of detection is 2 ppm; the result of limit of quantification is 7 ppm.
In the stability tests, farnesol beauty hydrogel patch was placed in the room temperature condition (25 ± 2 ℃) and the accelerated condition (40 ± 2 ℃) for six-month stability test. The appearance of product did not significantly change and the content of farnesol was declined to 92.78 ％ in the room temperature test and declined to 88.01 ％ in the accelerated test at the six month.

摘要………………………………………………………………………………I
Abstract…………………………………………………………………………II
致謝……………………………………………………………………………IV
目錄……………………………………………………………………………VI
表目錄………………………………………………………………………VIII
圖目錄…………………………………………………………………………IX
第一章、 緒論
一、 簡介……………………………………………………………………1
二、 研究目的………………………………………………………………3
三、 主要成份介紹…………………………………………………………5
第二章、 實驗
一、 藥品……………………………………………………………………22
二、 儀器設備………………………………………………………………23
三、 氣相層析儀原理及簡介………………………………………………24
四、 氣相層析儀之分析條件………………………………………………33
五、 G C 分析方法之確效…………………………………………………39
六、 水膠貼布的製作………………………………………………………43
七、 美容水膠貼布(含1%金合歡醇)的製作………………………………43
八、 空白水膠貼布的製作…………………………………………………45
九、 不同溫度及時間對水膠貼布的影響…………………………………45
十、 標準品與內標品溶液配製……………………………………………46
十一、 水膠貼布中成份萃取法………………………………………………47
十二、 成份含量的計算………………………………………………………47
第三章、 結果與討論
一、 G C 分析方法之確效…………………………………………………48
1. 專一性(specificity)…………………………………………………………48
2. 精密度(precision)…………………………………………………………56
3. 線性(linearity)………………………………………………………………59
4. 準確度(accuracy)…………………………………………………………61
5. 偵測極限、定量極限………………………………………………………62
6. 分離因子之導出結果………………………………………………………62
二、 不同時間對美容水膠貼布濃度的影響………………………………63
三、 不同時間對美容水膠貼布外觀的影響………………………………67
第四章、 結論……………………………………………………………68
第五章、 參考文獻………………………………………………………70

表目錄

表一：烘箱升溫程序…………………………………………………………38
表二：水性藥膠布主要成份…………………………………………………44
表三：標準品與美容水膠貼布成份滯留時間之數據………………………48
表四：Farnesol的波峰面積重複性實驗(第一天) ……………………………56
表五：Farnesol的波峰面積重複性實驗(第二天) ……………………………57
表六：Farnesol的波峰面積重複性實驗(第三天) ……………………………58
表七：使用於標準檢量線之Farnesol數據……………………………………60
表八：添加Farnesol之水性藥膠布回收率……………………………………61
表九：Farnesol之偵測極限與定量極限………………………………………62
表十：分離因子………………………………………………………………62
表十一：金合歡醇在25℃及40℃的環境下，6個月間的含量變化…………63
表十二：金合歡醇在25℃時的安定性數據…………………………………65
表十三：金合歡醇在40℃時的安定性數據…………………………………66
表十四：水膠貼布在25℃及40℃的環境下，6個月間的顏色與外觀變化…67

圖目錄

圖1：GC裝置圖………………………………………………………………25
圖2：GC注射系統示意圖……………………………………………………27
圖3：GC注射系統之注射孔…………………………………………………27
圖4：GC系統之分離管柱……………………………………………………29
圖5：本論文所使用的管柱尺寸與廠牌………………………………………29
圖6：火焰離子化檢測器………………………………………………………31
圖7：此為Agilent之分析圖譜，金合歡醇的波峰為18a、18b，在22分鐘左右出現…33
圖8：利用Agilent公司所提供方法之層析圖…………………………………34
圖9：Hyeunjoo Lee等人發表論文之分析圖………………………………… 35
圖10：仿照圖(9a)之方法圖譜…………………………………………………36
圖11：仿照圖(9b)之方法圖譜…………………………………………………36
圖12：自製水膠貼布…………………………………………………………45
圖13：金合歡醇300ppm標準品溶液之分析圖譜…………………………48
圖14：接近300ppm的自製的水性藥膠布稀釋樣品溶液之分析圖譜……49
圖15：空白貼布萃取空白層析圖譜…………………………………………49
圖16：專一性樣品溶液A(未破壞)氣相層析圖譜……………………………50
圖17：專一性樣品溶液B(加熱)氣相層析圖譜……………………………51
圖18：專一性樣品溶液C(酸化)氣相層析圖譜……………………………52
圖19：專一性樣品溶液D(鹼化)氣相層析圖譜……………………………53
圖20：專一性樣品溶液E(氧化)氣相層析圖譜……………………………54
圖21：此圖為H2O2標準溶液之氣相層析圖譜……………………………54
圖22：專一性樣品溶液F(紫外光照射)氣相層析圖譜……………………55
圖23：金合歡醇標準品三重複注射之檢量線圖……………………………59
圖24：金合歡醇在25℃及40℃的環境下，6個月間含量變化曲線圖………64

1.Yang Huijun1, GC-MS Analysis of Cymbidium ensifolium Volatile Components 2011,27(16):104-109.

2.http://zh.wikipedia.org/zh-tw/%E8%8B%A7%E7%83%AF.


3.Fahlbusch, Karl-Georg; Franz-Josef Hammerschmidt, Johannes Panten, Wilhelm Pickenhagen, Dietmar Schatkowski, Kurt Bauer, Dorothea Garbe, Horst Surburg. "Flavors and Fragrances" in Ullmann''s Encyclopedia of Industrial Chemistry. Wiley-VCH, Weinheim. 2002.

4.Cyclone Power to Showcase External Combustion Engine at SAE Event, Green Car Congress, 20 September 2007.

5.EPA R.E.D. Fact Sheet on Limonene, September 1994.

6.IARC Monographs on the evaluation of carcinogenic risks to humans 1999, 73-16, 307-27.

7.Crowell PL. Prevention and therapy of cancer by dietary monoterpenes. J. Nutr.. 3 1999, 129 (3): 775S–778S. PMID 10082788.

8.Tsuda H, Ohshima Y, Nomoto H, et al. Cancer prevention by natural compounds. Drug Metab. Pharmacokinet.. 8 2004, 19 (4): 245–63. PMID 15499193.

9.http://en.wikipedia.org/wiki/Triethanolamine

10.Klaus Weissermel, Hans-Jurgen Arpe, Charlet R. Lindley, Stephen Hawkins. Chap. 7. Oxidation Products of Ethylene. Industrial Organic Chemistry. Wiley-VCH. 2003: 159–161. ISBN 3527305785.



11.Sohoni, S.; R. Sridhar, G. Mandal. Effect of grinding aids on the fine grinding of limestone, quartz and portland cement clinker. Powder Technology. 1991, 67 (3): 277–286.


12.http://en.wikipedia.org/wiki/ Glycerol.

13.http://en.wikipedia.org/wiki/Castor_oil.

14.http://en.wikipedia.org/wiki/Polysorbate_20.

15.http://baike.baidu.com/view/2710321.htm.

16.http://en.wikipedia.org/wiki/Propylparaben

17.http://en.wikipedia.org/wiki/Sodium_polyacrylate .

18.What are the components of a typical disposable diaper?", Frequently Asked Questions about Disposable Diapers. The Disposable Diaper Net (Richer Investment Diaper Consulting Services). Accessed 29 April 2009.

19.History of Super Absorbent Polymer Chemistry, M2 Polymer Technologies, Inc. Accessed 29 April 2009.

20.鍾文彬，「3-1-Menthoxypropane-1,2-diol 在水性藥膠布中之安定性研究」，碩士論文，朝陽科技大學應用化學研究所，台中 (2008).

21.GC/MS Identification of Flavor and Fragrance Allergens in Some Common Snack Foods Using an Agilent J&W DB-17ms Capillary GC Column.

22.V. K. Raina, S. C. Verma, Sangeeta Dhawan,M. Khan, S.Ramesh, S. C. Singh, Anju Yadav and S. K. Srivastava ，Essential oilcomposition of Murraya exotica from the plains of northern India Flavour Fragr. J. 2006; 21: 140–142.


23.Omprakash H. Nautiyal, Krishna K. Tiwari，Extraction of Ambrette seed oil and isolation of Ambrettolide with its Characterization by 1H NMRVol. 4(2011): 75-80 .

24.ZHAO Zhen-dobg , SU Wen-qiang , CHEN Feng-yu , BI Liang-wu PROGRESS OF RESEARCHES ON RESOURCES AND BIOACTIVE APPLICATIONS OF FARNESOL. Vol. 25 Supplement Oct. 2005 .

25.R. Kennedy Keller , Rapid synthesis of isoprenoid diphosphates and their isolation in one step using either thin layer or flash . chromatography. Journal of Chromatography, 645 (1993) 1 6 1-167.

26.Thomas L. Horn , Lina Longa, Michael J. Cwik , Robert L. Morrissey , Izet M. Kapetanovic , David L. McCormick , Modulation of hepatic and renal drug metabolizing enzyme activities in rats by subchronic administration of farnesol. Chemico-Biological Interactions 152 (2005) 79–99.

27.Jean-Baptiste Roullet , Renee L. Spaetgens , Terry Burlingame , Zhong-Ping Feng , and Gerald W. Zamponi , Modulation of Neuronal Voltage-gated Calcium Channels by Farnesol. Vol. 274, No. 36, Issue of September 3, pp. 25439–25446, 1999.

28.Robert J. Lutz , Teresa M. McLain , and Michael Sinensky , Feedback Inhibition of Polyisoprenyl Pyrophosphate Synthesis from Mevalonate in Vitro. Vol. 267 No. 12 Issue of April 25, pp. 7983-7986 1992.

29.Farnesol-derived Dicarboxylic Acids in the Urine of Animals Treated with Zaragozic Acid A or with Farnesol. Vol. 272, No. 14, Issue of April 4, pp. 9197–9203, 1997.

30.Hyeunjoo Lee , Steven Finckbeiner , Characterization of (E,E)-farnesol and its fatty acid esters from anal scent glands of nutria (Myocastor coypus) by gas chromatography–mass spectrometry and gas chromatography–infrared spectrometry. Journal of Chromatography A, 1165 (2007) 136–143.