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研究生:李坤泰
研究生(外文):Kun-Tai Li
論文名稱:螢光性液相層析法對尿液中amphetamine、methamphetamine、MDMA、MDA及MDEA之高感度分析研究
論文名稱(外文):High sensitive analysis of amphetamine, methamphetamine, MDMA, MDA and MDEA in urine by fluorimetric-HPLC
指導教授:柯黃盛柯黃盛引用關係
指導教授(外文):Hwang-Shang Kou
學位類別:碩士
校院名稱:高雄醫學大學
系所名稱:藥學研究所碩士班
學門:醫藥衛生學門
學類:藥學學類
論文種類:學術論文
論文出版年:2006
畢業學年度:94
語文別:中文
論文頁數:82
中文關鍵詞:安非他命甲基安非他命液相層析
外文關鍵詞:HPLCamphetaminemethamphetamineMDMAMDAMDEA
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安非他命類藥物 amphetamine、methamphetamine、3,4-methylene- dioxymethamphetamine (MDMA)、3,4-methylenedioxyamphetamine (MDA) 與methylenedioxyethylamphetamine (MDEA) 因具有很強的中樞神經系統興奮及狂喜效果,近年來相當廣泛地被青少年所濫用,但因其對中樞神經系統及身體會產生嚴重的傷害,因此如何有效偵測此類藥物是一重要的課題。本研究主要的目的為利用螢光性衍生化液相層析法對人體尿液中安非他命類藥物建立一個簡單、快速及高感度分析檢測方法。本研究使用 (2-naphthoxy)acetyl chloride (NAC) 為螢光性衍生試劑,與安非他命類藥物進行衍生反應,使其產生具有螢光性之衍生物,然後配合高效能液相層析分離及螢光檢測器檢測分析 (螢光之激發光波長為229 nm,發散光波長為345 nm)。對於影響安非他命類藥物衍生反應之重要因素,包含衍生試劑濃度、borate buffer濃度及pH值、反應溫度與時間等條件,皆詳加探討。本法對添加於人體尿液中安非他命類藥物的分析檢測範圍為20 ~ 800 ng/mL,檢測極限為4 ng/mL (S/N=3,注射體積10 ?尳),應用本法於實際藥物濫用者的尿液分析,證實是可行的。
Amphetamine analogues amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylene- dioxyamphetamine (MDA) and methylenedioxyethylamphetamine (MDEA) have become popular drugs of abuse in recent year, because they are powerful stimulants of the central nervous system and serious injure to the human body. A simple, rapid and sensitive derivatization and fluorimetric-liquid chromatographic method is described for the determination of amphetamine analogues in human urine. The method is based on the derivatization of the amphetamine analogues from urine samples with (2-naphthoxy)acetyl chloride (NAC). The resulting naphthoxy derivatives were analyzed by liquid chromatography with fluorimetric detection (excitation wavelength 229 nm, emission wavelength 345 nm). Several parameters affecting the derivatization of amphetamine analogues were discussed including the concentration of derivatization reagent, concentration and pH value of borate buffer, reaction temperature and reaction time. The linear range of the method for the determination of amphetamine analogues derivatives were 20 ~ 800 ng/mL. The detection limit of amphetamine analogues derivatives were reach 4 ng/mL (S/N = 3, injected amount 10 ?尳). Application of the method to the analysis of amphetamine analogues in drug abuser’s urine proved feasible.
中文摘要 iv
英文摘要 v
圖目錄 vi
表目錄 viii
第壹章 緒論 1
第貳章 實驗部份 8
一、 試藥與材料 8
二、 儀器 10
三、 衍生試劑(2-Naphthoxy)acetyl chloride (NAC) 之合成與精製 11
四、 試劑溶液之配製 13
五、 高效能液相層析之分析條件 15
六、 氣相層析-質譜法 (Gas chromatography-Mass spectrometry, GC-MS) 之分析條件 16
七、 Amphetamine、Methamphetamine、MDMA、MDA、MDEA與Ketamine衍生物之合成及結構探討 18
八、 Amphetamine、Methamphetamine、MDMA、MDA與MDEA適當衍生反應條件之探討 20
1. 衍生試劑濃度之探討 21
2. Borate buffer濃度之探討 22
3. Borate buffer pH值之探討 23
4. 反應溫度與時間之探討 24
九、 人體尿液中衍生物安定性 25
十、 檢量線之建立及精密度與準確度之探討 25
1. 檢量線之建立 25
2. 同日內分析(Intra-day) 26
3. 異日間分析(Inter-day) 27
十一、 應用分析 27
第參章 結果與討論 29
一、 Amphetamine、Methamphetamine、MDMA、MDA、MDEA與Ketamine衍生物之合成及結構確認 29
二、 高效能液相層析條件最佳化探討 43
三、 內部標準品的選擇 48
四、 最適當衍生反應條件之建立 49
1. 衍生試劑濃度之探討 52
2. Borate buffer濃度之探討 53
3. Borate buffer pH值之探討 54
4. 反應溫度與時間探討 55
五、 衍生物之安定性 58
六、 檢量線之建立及其精密度與準確度之測定法 59
1. 檢量線之建立 59
2. 精密度及準確度之測定 60
七、 應用分析 62
第肆章 結論 64
第伍章 參考文獻 66
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