一滴溶劑微萃取法連結大氣壓基質輔助雷射脫附質譜法於多巴胺與短桿菌抗生素之分析及利用電灑質譜研究奈米鐵粒子表面所吸附之水分子團簇

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Title:	一滴溶劑微萃取法連結大氣壓基質輔助雷射脫附質譜法於多巴胺與短桿菌抗生素之分析及利用電灑質譜研究奈米鐵粒子表面所吸附之水分子團簇
Other Titles:	Combining single drop solvent microextraction with atmospheric pressure matrix assisted laser desorption/ionization mass spectrometry for analysis of dopamine and gramicidin A and physical adsorption of nanoscale cages of water clusters on the surfaces of iron nano-particles investigated by electrospray / ion trap tandem mass spectrometry
Authors:	林其賢;Lin, Chi-hsien
Contributors:	淡江大學化學學系碩士班吳彗芬;Wu, Hui-fen
Keywords:	一滴溶劑微萃取法;大氣壓基質輔助雷射脫附質譜法;電噴灑質譜法;Single-Drop Solvent Microextraction (SDSME);Atmospheric Pressure Matrix Assisted Laser Desorption/Ionization (AP-MALDI);ElectroSpray Ionization(ESI)
Date:	2005
Issue Date:	2010-01-11 02:47:06 (UTC+8)
Abstract:	大氣壓下基質輔助雷射脫附質譜法與電噴灑質譜法是近年發展出來的軟性游離法，本論文利用此二種游離法來研究目前相當熱門的藥物分析、生化分子定序以及於奈米鐵粒子的研究。本論文共分成兩部份，第一部分，一滴溶劑微萃取（SDME）是近年來發展起來的一種新型的樣品前處理技術，該技術集採樣、萃取和濃縮於一體，需要有機溶劑量非常少，是一種對人體及環境傷害極低的萃取技術。本實驗利用一滴溶劑微萃取法結合大氣壓基質輔助雷射脫附游離法（SDME/AP-MALDI）分析水中、尿液、血清中多巴胺與短桿菌抗生素，並探討萃取因子對萃取效率的影響。這些萃取因子包括了溶劑種類選擇、pH 值調控、磁石攪拌速度、萃取時間、鹽類添加濃度。一滴溶劑微萃取法結合大氣壓基質輔助雷射脫附游離法來分析多巴胺與短桿菌抗生素的偵測極限分別低於80ng/mL 與20ng/mL，本實驗目的在利用萃取溶劑對多巴胺及短桿菌抗生素的專一性以降低水及體液中的基質干擾，並且以最快速與簡單的實驗步驟達到分析各種體液中的多巴胺與短桿菌抗生素，進而利用串聯質譜分析其結構。第二部份，奈米粒子於電噴灑質譜法的研究，近年來，不論是實驗或是理論計算對於水分子團簇的研究多有著墨。本實驗為首次使用電噴灑游離法搭配高次串聯質譜來研究奈米鐵粒子於水中以及各種不同的有機溶劑中所產生的水分子團簇。 This thesis includes two projects. In the first project, a novel technique of direct combining single drop micro-extraction (SDME) with atmospheric pressure matrix assisted laser desorption/ionization(AP-MALDI) in an ion trap tandem mass spectrometer has been demonstrated for rapid analysis of dopamine and gramicidin A in aqueous solution, human urine and plasma. The effects of the solventselection, extraction time, sample agitation rate, sample pH values and matrix concentration on the extraction efficiency were examined. The limits of detection (LOD) of the SDME/AP-MALDI/MS experiment were in the range of 50 to 80 and 0.5 to 20 ng/mL for dopamine and gramicidin A,respectively. The SDME/AP-MALDI/MS/MS experiments were also performed to elucidate the structures of dopamine and mapping the sequence for gramicidin A. This method is not only simple,rapid and efficient but also can greatly reduce the interferences in human urine and plasma. In the second project, a very interesting phenomenon was observed from physical adsorption of nanoscale cages of water clusters of [(H2O)20O]+ (m/z 376) and [(H2O)21+H3] + (m/z 381) on the surface of iron nano-particles probed by electrospray / ion trap tandem mass spectrometry. The assignments and structures of these water cluster ions were investigated by using MS/MS and MS3 experiments. This study has revealed that the iron nano-particles exhibit very strong physical adsorption capability for the nanoscale cages of water cluster ions on the surface of the iron nano-particles.
Appears in Collections:	[Graduate Institute & Department of Chemistry] Thesis

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