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研究生:陳盈成
研究生(外文):In-Chen Chen
論文名稱:利用液相層析/質譜儀檢測吳茱萸之四個生物鹼
論文名稱(外文):Determination of Four Alkaloids in Evodia rutaecarpa by Liquid Chromatography-Electrospray Ionization Mass Spectrometry
指導教授:游錫榕游錫榕引用關係
指導教授(外文):Professor Hsi-Jung Yu
學位類別:碩士
校院名稱:中國文化大學
系所名稱:應用化學研究所
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:2001
畢業學年度:89
語文別:中文
論文頁數:59
中文關鍵詞:吳茱萸液相層析質譜儀
外文關鍵詞:Evodia rutaecarpaLiquid Chromatography Mass Spectrometry
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吳茱萸的未成熟果實中含四種主要的活性化合物(synephrine,dehydroevodiamine,evodiamine,rutaecarpine)。其分別被証實具有不同的生物活性,相當具有研究價值。對其之分析研究報告相當多,但始終未有使用液相層析/質譜儀(liquid chromatography/mass,LC/MS)對其定性及定量之研究報告。
本實驗使用C-18的逆向層析管柱及梯度流析(gradient elution)的方法作分離。Mass部分是以選擇離子形式(selected ion monitoring,SIM)作為質譜偵測模式。
本實驗也對吳茱萸之分離條件進行探討,即移動相(mobile phase)加入的酸濃度、種類及沖提流速對化合物質譜peak的abundance之影響。藉而使其分離效果提升。
使用3-methoxyrutaecarpine作為internal standard,四個化合物的calibration curve的濃度範圍為0.1~ 8.0 ppm,線性(linear)為r2≧0.996,RSD(%)為1.1~12.9,accuracy(%)為72 ~126。
實驗結果顯示吳茱萸以1:0(MeOH/H2O)條件萃取之粗抽液經檢測四個化合物(synephrine,dehydroevodiamine,evodiamine,rutaecarpine)含量分別為0.43、7.76、1.72、2.93(mg/g);吳茱萸以1:1(MeOH/H2O)條件萃取之粗抽液經檢測四個化合物含量分別為2.06、5.31、0.48、0.64 (mg/g);臭辣樹以1:0(MeOH/H2O)條件萃取之粗抽液經檢測四個化合物含量分別為0.15、0.55、1.18、1.10(mg/g),臭辣樹以1:1(MeOH/H2O)條件萃取之粗抽液經檢測四個化合物含量分別為0.17、0.61、0.08、0.30 (mg/g)。
A liquid chromatography-eletrospray mass spectrometry (LC-ES-MS) method has been developed for the direct and rapid analysis of four alkaloids in a crude extract of the dried fruit of Evodia rutaecarpa. A C18 column and a gradient elution were employed for the separation. Selective ion monitoring [M+1]+ (m/z=168 for synephrine (1), m/z=302 for dehydroevodiamine (2), m/z=304 for evodiamine (3), and m/z=288 for rutaecarpine (4)) was utilized for quantitative measurement and internal standard was 3-methoxyrutaecarpine. The standard curves of four alkaloids were linear (> 0.996) over the concentration range of 0.1- 8.0 ng/mL. The relative standard deviations of four alkaloids ranged between 2.5 — 12.9 % (intraday) and 0.6 — 11.9 % (interday). The limit of detection of the method is 0.1 ppm of 1, 0.005 ppm of 2, 0.05 ppm of 3, and 0.03 ppm of 4 per injection, respectively. When this LC/MS method was applied to the 100% methanol extract of Evodia rutaecarpa, the contents of the four alkaloids were 1 0.43 mg, 2 7.76 mg, 3 1.72 mg, and 4 2.93 mg per gram, respectively. Also, the contents of the four alkaloids from 50% methanol extract of Evodia rutaecarpa were 1 2.06 mg, 2 5.31 mg, 3 0.48 mg, and 4 0.64 mg per gram, respectively.
目錄
________________________________________________________________
中文摘要 i
英文摘要 iii
壹、緒論
1-1. 吳茱萸簡介 1
1-2. LC/MS 簡介 3
1-3. LC/MS 之分析過程及原理 7
貳、儀器與材料
2-1. 儀器設備 14
2-2. 藥品試劑 15
參、實驗部分
3-1. 吳茱萸及臭辣樹之樣品萃取 16
3-2. MS 的條件 19
3-3. HPLC 的分離條件 20
3-3-1. 同種類及濃度之酸對各活性化合物sensitivity
的影響
3-3-2. Mobile phase的梯度流析條件
3-3-3. Mobile phase沖提流速對四個活性化合物abundance
的影響
3-4. Collision induced dissociation 24
3-5. Calibration curve 25
3-6. Accuracy and precision 26
3-7. Limit of detection and limit of quantity 28
3-8. 吳茱萸及臭辣樹之定量 29
肆、結果與討論
4-1. 分離部分 30
4-2. Collision induced dissociation 38
4-3. 吳茱萸及臭辣樹在不同萃取液比例下之含量 40
4-4. Calibration curve 42
4-5. Accuracy and precision 46
4-6. Limit of detection and limit of quantity 47
伍、參考文獻 55
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