溶劑微萃取（SME）是近年來發展起來的一種新型的樣品前處理技術，此種新方法具有快速、簡單、經濟、有效率而且需要有機溶劑量非常少，是一種符合環保的萃取技術。本論文共分成兩部份，在第一個實驗，首次利用微量吸管進行液相微萃取法並結合大氣壓基質輔助雷射脫附游離/離子阱質譜儀（AP-MALDI/ITMS），並對溶劑種類選擇、基質濃度、萃取時間、磁石攪拌速度、鹽類添加濃度、pH值調控等因子探討，以最快速與簡單的實驗步驟達到分析尿液和血液中的三環抗憂鬱藥物（Nortriptyline），而於水中、尿液和血液中的偵測極限分別可達10、50和100 ng/mL，並且利用串聯質譜進行定性分析。在第二個實驗，利用一滴溶劑微萃取法萃取一滴溶液結合氣相層析質譜儀（DDSME/GC/MS），並且利用自身離子/分子反應（SIMR）與高次串聯質譜的方法區別甲氧基苯乙酮同分異構物，且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、萃取時間、鹽類添加濃度。本實驗目的在利用這種新型的樣品前處理技術在只使用最少量的樣品與溶劑、最快速、簡便的步驟下完成同分異構物的鑑定。 Solvent microextraction is a novel sample preparation technique, this new method has the advantages of high extraction speed, simplicity, inexpensive and solvent-less.This thesis includes two projects. In the first project, liquid microextraction was performed by micropipette with tips and directly coupled to atmospheric pressure matrix assisted laser desorption/ionization ion trap tandem mass (AP-MALDI/MS/MS) for rapid analysis of nortriptyline from human urine and plasma. The effects of the solvent selection, matrix concentration, extraction time, agitation rate, salt concentration and sample pH values on the extraction efficiency were optimized. Detection limit of the MP-LPME/AP-MALDI/ITMS experiment was in the range of 10 to 100 ng/mL for nortriptyline. In the second project, a novel sample pretreatment technique termed drop-to-drop solvent microextraction (DDSME) coupled with gas chromatography/self-ion molecule reaction and tandem mass spectrometry (GC/SIMR/MS/MS/MS) to differentiate methoxyacetophenone isomers.
