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研究生:林士為
研究生(外文):Shih-wei Lin
論文名稱:線上固相萃取結合液相層析質譜儀檢測尿液中氟硝西泮類藥物
指導教授:傅明仁
指導教授(外文):Ming-ren Fuh
學位類別:碩士
校院名稱:東吳大學
系所名稱:化學系
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:2005
畢業學年度:93
語文別:中文
論文頁數:121
中文關鍵詞:氟硝西泮線上固相萃取
相關次數:
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氟硝西泮(Flunitrazepam)俗稱強姦藥片;為國內青少年濫用作為強姦及自殺犯罪工具。吸食後會很快地以代謝物氨基氟硝西泮(7-Aminoflunitrazepam)之型式排出;故檢測此藥物在尿中之殘留可作為是否吸食之指標。許多偵測氟硝西泮類藥物的方法已經開發出,但步驟多為繁瑣。本論文將介紹以線上固相萃取(On-line Solid Phase Extraction)/液相層析/電灑質譜儀檢測尿液中的氨基氟硝西泮(7-Aminoflunitrazepam)、去甲基氟硝西泮(N-desmethylflunitrazepam)
、氟硝西泮(flunitrazepam)的基質干擾並檢測其含量之分析方法。
本研究利用乙晴沉澱尿液中的蛋白質,以線上固相萃取結合液相層析電灑質譜儀檢測尿液基質對樣品的干擾。本方法之固相萃取管柱為HLB mixed mode結合C8逆相層析分析管柱同步進行分離。以二次質譜(MS/MS)和D4-N-desmethylflunitrazepm作為內標準品進行定量,兩段檢量線(20-200和200-2000 ng/ml)可以得到很好的定量結果。各分析物的檢測極限約為1 ng/ml,回收率為95.1%~101.2%。本論文亦將討論此新分析方法應用於疑似服用藥物者尿液樣品之檢測結果經過;經過和氣相層析質譜法結果相對差異度為2.7%~84.2%。
目 錄
中文摘要 頁次
圖目錄
表目錄
第一章 緒論 1
第一節 氟硝西泮藥物之介紹 1
第二節 利用線上固相萃取結合液相層析/電灑/質譜
檢測尿液中之氟硝西泮藥物 6
第三節 液相層析電灑質譜儀 7
第四節 離子阱質譜儀 13
第二章 實驗部份 18
線上固相萃取結合液相層析電灑質譜檢測尿液中氟
硝西泮類藥物 18
第一節 樣品及試劑 18
第二節 儀器及設備 18
第三節 實驗架構 20

第三章 結果與討論 38
線上固相萃取結合液相層析電灑質譜檢測尿液中氟硝
西泮類藥物 38
第一節 離子阱質譜儀部分 38
1-1. 質譜儀毛細管出口端電壓對訊號強度的影響 38
1-2. 質譜儀斷裂電壓對訊號強度的影響 40
第二節 液相層析質譜儀部分 40
2-1. 氟硝西泮類藥物初步分離 50
2-2. 添加劑對電灑質譜儀的影響 50
第三節 線上固相萃取部分 51
3-1. 固相萃取條件之測試 51
Ⅰ活化步驟探討
Ⅱ注入液探討
Ⅲ沖洗液一探討
Ⅳ沖洗液二探討
3-2. 線上固相翠取管柱與液相層析管柱連結之討
論 62
第四節 基質效應於尿液樣本之探討 66
4-1. 液相萃取結合線上固相萃取液相層析電灑質譜
儀 66
4-2. 尿液的蛋白質沉澱探討 66
(4-3. 氟硝西泮類藥物經線上固相萃取於液相層析
管柱的分離分離之探討 68
4-4. 離子抑制效應的評估 77
第五節 線上固相萃取連結液相層析質譜儀 79
5-1. 線性關係與偵測極限 79
5-2. 精確度與準確度之評估 81
第六節 真實樣本中氟硝西泮藥物之檢測 85
第七節 結論 102

第四章 參考文獻 104
附錄:質譜儀霧化條件
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