林震煌Lin, Cheng-Huang賴珮華Lai, Pei-Hua2019-09-04不公開2019-09-042015http://etds.lib.ntnu.edu.tw/cgi-bin/gs32/gsweb.cgi?o=dstdcdr&s=id=%22G060242017S%22.&%22.id.&http://rportal.lib.ntnu.edu.tw:80/handle/20.500.12235/99963本研究利用靜電紡絲法(electrospinning)製造出排列方式及不同特性的纖維薄膜,取代傳統紙片電噴灑(paper-spray)質譜法中使用的層析濾紙,以數種藥物探討不同纖維材質對電噴灑效果及偵測靈敏度的影響。實驗分別以聚乳酸、聚偏二氟乙烯、尼龍以及聚碳酸酯製成纖維薄膜。這些高分子材料先溶解於有機溶劑中,利用高電壓做為驅動力,經電噴灑紡頭以電噴灑方式射出纖維絲後,再由高速收集滾筒匯集成薄膜。薄膜的厚度約在20 μm 之內。此外,為探討纖維排列對偵測靈敏度的影響,利用不同構造的電噴灑紡頭,分別製成各式規則與不規則排列纖維薄膜進行比較。再者,當單層薄膜的厚度為奈米等級時,由於缺少韌性及足夠的強度支撐,遇到有機溶劑時容易變形捲曲而無法使用。為了克服此一缺點,本研究發展以鋁箔紙支撐的各式超薄的陣列多孔中空纖維膜,不僅可以穩定電噴灑現象,也不容易變形。實驗結果發現,各式薄膜當中,以聚乳酸製成的厚度超薄、表面平滑、具規則排列的纖維其電噴灑效果最好。究其原因可能是表面規則排列且厚度薄的纖維,可以有效的提升溶劑攜帶樣品的傳輸效率。在相同質譜條件之下,比起傳統使用的層析濾紙,偵測極限降低一個數量級。除此之外,為了更增加靈敏度,以市售聚丙烯中空纖維,先進行液-液微萃取之後,再將中空纖維的一端裁切成25 度尖端斜口的形狀,直接作為紙片-電噴灑的游離源進行檢測。結果發現,配合液-液微萃取的步驟,更低濃度的分析物可以有效的被萃取出來,降低偵測極限,提高靈敏度。實驗發現在相同質譜條件之下,比起傳統使用的層析濾紙法,偵測極限幾乎降低~2 個數量級。本研究也針對尿液中添加的藥物進行檢測,皆可快速並準確的鑑定分析樣品。Various types of membranes, the so-called array porous hollow fibers, were synthesized and used in paper-spray mass spectrometry (PS-MS). By using several abused drugs as the test samples, the ionization efficiencies and the limit of detections were investigated when the different types of membranes were used. For making these membranes, polymer of poly-L-lactic acid (PLLA), polyvinylidene fluoride (PVDF), nylon and polycarbonate (PC) were dissolved in organic solvents, respectively, and then by means of electrospinning technique, the fibers can be collected on a high speed roller, leading to form a piece of membrane. Thickness of these membranes was within 20 μm. In addition, it is found out from the research that using aluminum foil to support fiber can not only stabilize electric spray phenomenon but also make the fiber not easy deformed. The findings show that the limit of detection can be dramatic improved when PLLA was used which is the best of all. This is because PLLA is very toughness and extremely thin, leading to the sample solution much easier ejected and ionized toward the mass inlet. Under the same MS conditions, the detection limit improve one order than the use of the chromatography paper. And after the liquid-liquid microextraction process, one of the end of the hollow fiber was cut into a bevel-shaped, and then using directly for electrospray ionization. The findings show that the limit of detection can be improved ~ 2 orders. Detailed information and the use the technique in the analysis of a urine sample are reported.紙片-電噴灑質譜法靜電紡絲法中空纖維液-液微萃取paper-spray/MSelectrospinninghollow fibersliquid-liquid microextraction多孔中空纖維薄膜的合成與其電噴灑/質譜法上之應用The synthesis of array porous hollow fiber membranes and its applications in electrospray ionization/mass spectrometry