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文氏管電噴灑游離質譜法的開發 = Development of Vent...

國立高雄大學應用化學系碩士班

文氏管電噴灑游離質譜法的開發 = Development of Venturi Electrospray Ionization Mass Spectrometry

紀錄類型:	書目-語言資料,印刷品 : 單行本
並列題名:	Development of Venturi Electrospray Ionization Mass Spectrometry
作者:	楊瑞崎,
其他團體作者:	國立高雄大學
出版地:	[高雄市]
出版者:	撰者;
出版年:	2013[民102]
面頁冊數:	114面圖，表格 : 30公分;
標題:	文氏管效應
標題:	online
電子資源:	http://handle.ncl.edu.tw/11296/ndltd/01497440297871337206
附註:	參考書目：面97-101
附註:	102年10月31日公開
摘要註:	本研究應用文氏管效應(Venturi effect)開發一項可以進行線上即時分析化合物的簡易質譜法，此項方式命名為文氏管電噴灑游離質譜法(Venturi electrospray ionization mass spectrometry, VESI-MS)。使用VESI-MS時不需要加裝任何輔助設備就可以自動將樣品導入質譜儀的游離源中進行分析，而進樣方式可以採用單一進樣或是以T型連接方式進行雙重進樣。VESI-MS可應用於即時分析化學反應時化合物的生成變化，並觀測不同實驗條件對產物選擇性的影響，可以增加對反應機制的了解；VESI-MS也可以用來線上改變樣品的基質，達到增強分析物於電噴灑游離時的訊號。雖然電噴灑游離時泰勒錐(Taylor cone)的持續生成有可能會拖曳溶液，然而實驗證明霧化氮氣所形成的文氏管效應才是自動進樣的主因，以VESI-MS分析葡萄糖胺水溶液時，開啟或關閉電噴灑游離電壓時所記錄的流速依序為19.9±1.9 μL/min和18.7±1.1 μL/min，證實泰勒錐對樣品液的流動影響極小。樣品溶液的種類和輸送管內徑大小等參數皆會影響進樣流速的快慢，用於VESI-MS的PEEK管或毛細管長度分別須短於20公分和15公分才能自動進樣，而適用的輸送管的內徑介於75 μm 到250 μm之間。以VESI-MS探討cytochrome c水解反應機制時，可以觀察到KIFVQK胜肽斷片生成後才再繼續水解成IFVQK片段，顯示cytochrome c中不同位置lysine (K)的水解速率會因構型的影響而有顯著的不同。VESI-MS雙重進樣方式的研究，包含將醋酸水溶液線上添加入咖啡因樣品液中，因而提升了咖啡因訊號強度約55倍，並且降低了鹽類訊號的干擾。雙重進樣方式也可以應用於同分異構物的辨別，苯乙酮經Beckmann重排合成醯胺，可以得到acetanilide (AA)與N-methylbenzamide (NMB)兩種同分異構物，以雙重進樣裝置導入參考物acetaminophen (APAP)分別和AA或NMB標準品生成質子化二聚體，經碰撞誘導解離後斷片訊號強度比分別為IAA/IAPAP = 0.15和INMB/IAPAP = 4.17，利用此項數據進一步分析混合液中AA和NMB的相對含量其結果符合預期，未來可以使用VESI-MS線上即時分析不同反應參數對產物選擇性的影響。 A handy ionization method on the basis of Venturi effect was developed. The method was named as Venturi electrospray ionization mass spectrometry (VESI-MS). VESI-MS can self-pumping sample solution into the ion source of Q-TOF mass spectrometry. Sample inlet device of VESI-MS can be either single or dual inlets. VESI-MS can perform online study on organic reactions in real-time and investigated effects of experimental conditions on variation of products. Result will assist researchers to understand reaction mechanisms that interested. VESI-MS with dual inlets was applied for modification of matrix in sample solution to enhance analyte ionization efficiency or to perform kinetic method.Studies showed that nitrogen used as nebulization gas for ESI is the major driving force for self-pumping and formation of Taylor cone has only minor effect. Self-pumping flow rates of glucosamine solution are 19.9 ± 1.9 μL / min and 18.7 ± 1.1 μL / min for turning on or off capillary voltage, respectively. The self-pumping flow rate is affected by solvent used and diameter of tubing for transporting solution. Suitable diameter of transporting tubing is ranged from 75 μm to 250 μm and lengths of transporting tubing should be less than 20 cm and 15 cm for PEEK and capillary tubes, respectively.VESI-MS was demonstrated to investigate tryptic digestion of cytochrome c in real-time. Result showed that formation KIFVQK is more facile than that of IFVQK. The hydrolysis rate of lysine (K) is affected by its location on cytochrome c. VESI with dual inlets (T-VESI) was applied to improve signal intensity. Intensity of protonated caffeine is enhanced approximately 55 times after online adding acetic acid aqueous solution into sample solution via T-shape connector. Formation of sodiated caffeine cation is also suppressed. Moreover, T-VESI was combined with kinetic method to distinguish acetanilide (AA) and N-methylbenzamide (NMB). AA and NMB are isomeric products that generated from acetophenone via Beckmann rearrangement. T-VESI can be used for post-reactor mixing reference compound acetaminophen (APAP) and AA or NMB standard to perform kinetic method. Collision-Induced dissociation of proton-bound dimers generated showed that the relative intensities of fragments are IAA/IAPAP = 0.15 and INMB/IAPAP = 4.17. These data were applied to solve relative amount of AA and NMB in artificial sample and the result is inconsistent with expectation. The strategy can be used to investigate effect of reaction conditions on isomeric selectivity in the future.

文氏管電噴灑游離質譜法的開發 = Development of Venturi Electrospray Ionization Mass Spectrometry
楊, 瑞崎

文氏管電噴灑游離質譜法的開發 = Development of Venturi Electrospray Ionization Mass Spectrometry / 楊瑞崎撰 - [高雄市] : 撰者, 2013[民102]. - 114面 ; 圖，表格 ; 30公分.
參考書目：面97-101102年10月31日公開.
文氏管效應online

文氏管電噴灑游離質譜法的開發 = Development of Venturi Electrospray Ionization Mass Spectrometry
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