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研究生:王碧蓮
研究生(外文):Pi-Lien Wang
論文名稱:利用液相層析串聯質譜技術檢測水環境中藥物殘留物之方法開發與應用
論文名稱(外文):Determination of pharmaceutical resides in waters by solid phase extraction with liquid chromatography-tandem mass spectrometry
指導教授:丁望賢丁望賢引用關係
指導教授(外文):Wang-Hsien Ding
學位類別:碩士
校院名稱:國立中央大學
系所名稱: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:2005
畢業學年度:93
語文別:中文
論文頁數:106
中文關鍵詞:安妥明卡巴氮平液相層析串聯質譜技術那普洛辛凱妥普洛芬異布洛芬二克氯吩鈉固相萃取法
外文關鍵詞:ibuprofenLC-MS/MSdiclofenacketoprofennaproxenclofibric acidcarbamazepinesolid phase extraction
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近年來在環境檢測方面,科學家對於具有生物活性之微量藥物殘留在環境中的含量與流布之檢測,產生濃厚的興趣與關注,主要是由於這類殘留藥物對野生動物或水中魚類的生存產生極大的衝擊,透過食物鏈的途徑甚至可能會影響到人類的健康。這類殘留藥物主要包括止痛劑、脂質調節劑與抗生素等等。而本實驗將針對以下六種常見的藥物殘留物進行分析與研究:安妥明、卡巴氮平、二克氯吩鈉、異布洛芬、凱妥普洛芬與那普洛辛。
本研究的主要目的在發展一套快速、可靠、穩定的分析方法,研究這些藥物殘留物在國內水環境中的流布與含量,首先以液相層析質譜儀在不同的沖提流速下進行分離後,再搭配三種不同的游離源尋找最佳化的層析分離法與游離化條件,並且搭配良好的固相萃取法,可以達到濃縮與去干擾的目的。由實驗結果發現以LC沖提流速為0.2 ml/min,搭配ESI游離介面進行二次質譜法可得到較佳的感度,並且在最佳化的層析分離方法與游離條件之下,偵測極限可達到0.4~80 ng/L,檢量線r2值均大於0.994。並且搭配可靠的前處理方法對於民生廢污水與河流水樣進行檢測,檢測結果發現在民生廢污水與河流水樣當中皆可偵測到這六種藥物殘留物的存在,濃度最高可達963 ng/L,回收率為45~117%,RSD值均小於8.5%。
A method for the determination of selected pharmaceutical residues (clofibric acid, ibuprofen, carbamazepine, naproxen, ketoprofen and diclofenac) in various water samples was developed and validated. The contents of pharmaceutical residues in water samples were extracted by Oasis HLB solid-phase extraction (SPE). The analytes were then identified and quantitated by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Three ionization techniques, electrospray ionization (ESI), atmospheric pressure chemical ionization (APCI), and atmospheric pressure photoionization (APPI), were tested, while ESI in negative and positive modes (for carbamazepine) proved to be the most sensitive ionization method. Limits of quantitation (LOQ) were established between 2.0 to 200 ng/L in 250 mL of water sample. Intrabatch and interbatch precision with their accuracy at two concentration levels were also investigated. The selected analytes were detected in concentrations from 24 to 963 ng/L in wastewater treatment plant effluent and river water samples.
目錄
中文摘要 ------------------------------------------------------------------------Ⅰ
英文摘要 ------------------------------------------------------------------------Ⅱ
謝誌 ------------------------------------------------------------------------------Ⅲ
目錄 ------------------------------------------------------------------------------Ⅳ
表目錄 ---------------------------------------------------------------------------Ⅶ
圖目錄 ---------------------------------------------------------------------------Ⅸ
第一章 前言 ---------------------------------------------------------------------1
1-1研究源起 ------------------------------------------------------------------1
1-2研究目標 ------------------------------------------------------------------4
第二章 文獻回顧 ---------------------------------------------------------------6
2-1 藥物殘留物的來源 -----------------------------------------------------6
2-2 藥物殘留物在環境中的作用機制與影響 --------------------------6
2-3 分析物與相關文獻 -----------------------------------------------------8
2-3-1 分析物 ------------------------------------------------------------8
2-3-2 國外相關文獻 -------------------------------------------------10
2-4 固相萃取法 -------------------------------------------------------------16
2-5 液相層析質譜儀 -------------------------------------------------------19
2-5-1 電噴灑游離法 -------------------------------------------------20
2-5-2 大氣壓力化學游離法 ----------------------------------------22
2-5-3 大氣壓力光游離法 -------------------------------------------22
第三章 實驗步驟與樣品分析 -----------------------------------------------24
3-1 實驗藥品與儀器設備 -------------------------------------------------24
3-1-1 實驗藥品 -------------------------------------------------------24
3-1-2 儀器設備 -------------------------------------------------------26
3-2實驗步驟 -----------------------------------------------------------------27
3-2-1 標準品的製備 -------------------------------------------------27
3-2-2 標準品的測定 -------------------------------------------------28
3-2-3 萃取步驟 -------------------------------------------------------31
3-2-4 真實水樣萃取及淨化 ----------------------------------------32
第四章 結果與討論 -----------------------------------------------------------33
4-1 不同游離源在正負離子模式下之分析結果-----------------------33
4-2 液相層析儀之沖提流速對於不同離子源的影響-----------------38
4-2-1不同的沖提流速對APCI游離源之影響--------------------40
4-2-2不同的沖提流速對APPI游離源之影響--------------------42
4-2-3不同的沖提流速對ESI游離源之影響----------------------47
4-3 檢量線--------------------------------------------------------------------57
4-4 固相萃取-----------------------------------------------------------------59
4-5 真實水樣之分析結果--------------------------------------------------61
第五章 結論---------------------------------------------------------------------86
參考文獻--------------------------------------------------------------------------88
參考文獻
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