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研究生:林秋束
研究生(外文):Chiou-Shu Lin
論文名稱:液相層析質譜術於尿液中鎮靜安眠類及濫用藥物之偵測
論文名稱(外文):Liquid Chromatography-Mass Spectrometry for Determination of Sedative-Hypnotics and Abused Drugs in Urine
指導教授:李茂榮李茂榮引用關係
學位類別:碩士
校院名稱:國立中興大學
系所名稱:化學系所
學門:自然科學學門
學類:化學學類
論文種類:學術論文
畢業學年度:96
語文別:中文
論文頁數:107
中文關鍵詞:液相層析質譜術固相萃取法安眠藥濫用藥物
外文關鍵詞:LC/MSSPEsedative-hypnotic drugabused drug
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  • 被引用被引用:3
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本實驗探討以固相萃取法結合液相層析質譜術於高解析選擇反應偵測,利用加熱式電灑游離法正、負離子切換模式,同時偵測尿液中鎮靜安眠類及濫用藥物。並探討固相萃取吸附劑種類、緩衝溶液pH值、沖洗及沖提溶劑種類對萃取效果之影響,並討論此技術之線性範圍、偵測極限值及再現性等。
實驗結果顯示,以混合相SPEC MP3吸附劑之碟盤固相萃取管柱萃取1 mL尿液樣品,其活化過程依序加入0.5 mL甲醇、0.5 mL水及0.5 mL pH值為5.0之緩衝溶液,再分別以0.5 mL的水及5 %甲醇水溶液清洗後,以乙酸乙酯/異丙醇/氫氧化銨(78/20/2, v/v/v)1 mL進行兩次沖提後可得到較佳的萃取效果。除了phenobarbital的線性範圍為25~1000 ng/mL與偵測極限在0.8 ng/mL外,其於13種藥物之線性範圍均在0.05~50 ng/mL,偵測極限在0.001~0.1 ng/mL,線性相關係數皆在0.9907以上。實驗結果顯示以固相萃取法結合液相層析質譜術分析尿液中鎮靜安眠類及濫用藥物,可達到pg/mL程度,具有選擇性及靈敏度高之特性。將此方法應用至真實尿液樣品中可偵測到6.86 ng/mL之藥物含量,故本技術可以作為尿液中鎮靜安眠類及濫用藥物確認檢驗技術之參考。
A sensitive method for quantification and identification of sedative-hypnotics and abused drugs in human urine using solid phase extraction combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) with positive/negative exchange scan was evaluated in this study. The target sedative-hypnotics and abused drugs studied are including ketamine, norketamine, dehydronorketamine, zolpidem, zopiclone, zaleplon, 1-benzylpiperazine, clenbuterol, carisoprodol, alprazolam, lorazepam, midazolam, nimetazepam, and phenobarbital. The ionization method was performed by the heated electrospray ionization (HESI). The highly-selective reaction monitoring (H-SRM) was adopted to obtain high ionization efficiency and reduce the interference from the urine matrix. Disk solid phase extraction was used to extract trace analytes from urine matrices. The optimal parameters of solid phase extraction, such as sorbent materials, pH, washing and elution solvent were systematically studied. The linearity range was 0.05 to 1000 ng/mL. Limits of detection (LOD) of fourteen drugs were between 0.001 to 0.8 ng/mL. The correlation coefficients above 0.9907 were ontained. The proposed method offered the ng/mL level sensitivity and high selectivity for determination of sedative-hypnotics and abused drugs in human urine.
謝誌 I
中文摘要 II
英文摘要 III
目錄 IV
表目錄 VIII
圖目錄 IX

壹、緒論 1
1.1 前言 1
1.2 鎮靜安眠類及濫用藥物之介紹 2
1.3 鎮靜安眠類及濫用藥物之檢測分析方法 8
1.4 質譜儀儀器原理 9
1.4.1 電灑游離法 11
1.4.2 大氣壓化學游離法 15
1.4.3 串聯質譜儀 18
1.4.4 四極矩質量分析器之原理 20
1.5 固相萃取法 24
貳、實驗部分 32
2.1 標準品與試劑 32
2.2 藥品配製 33
2.2.1 玻璃器具之矽烷化 33
2.2.2 儲存標準溶液配製 33
2.2.3 內標準品溶液配製 34
2.2.4 用於正離子模式偵測之標準溶液配製 34
2.2.5 用於負離子模式偵測之標準溶液配製 35
2.2.6 含有分析物之尿液工作溶液配製 35
2.2.7 緩衝溶液配製 36
2.3 實驗器材及儀器設備 37
2.3.1 實驗器材 37
2.3.2 液相層析質譜儀 38
2.3.3 液相層析條件 39
2.4 固相萃取之實驗步驟 39
2.5 最佳化條件之探討 41
2.5.1 質譜儀離子源參數之探討 41
2.5.2 最佳離子化方法之探討 42
2.5.3 固相萃取法條件之探討 42
參、結果與討論 44
3.1 標準質譜圖譜之建立 44
3.2 選擇反應偵測之子代離子的選擇 48
3.3 液相層析質譜儀離子化參數之探討 61
3.4 液相層析質譜儀條件 62
3.5 液相層析儀之動相條件探討 64
3.6 最佳游離化法之探討 72
3.7 固相萃取法條件之探討 75
3.7.1 吸附劑種類之探討 75
3.7.2 緩衝溶液pH值之探討 76
3.7.3 沖洗溶劑之探討 81
3.7.4 沖提溶液種類之探討 84

3.8 以固相萃取法分析尿液中十四種鎮靜安眠類及濫用藥物之線性範圍、線性方程式、線性相關係數及偵測極限 88
3.9 以固相萃取法分析尿液中十四種鎮靜安眠類及濫用藥物之萃取回收率 91
3.10 以固相萃取法分析尿液中十四種鎮靜安眠類及濫用藥物之精密度 91
3.11 真實樣品中鎮靜安眠類及濫用藥物之偵測 93
肆、結論 98
伍、參考文獻 99
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