理學院: 化學研究所指導教授: 何國榮黃雅儒Huang, Ya-JuYa-JuHuang2017-03-022018-07-102017-03-022018-07-102015http://ntur.lib.ntu.edu.tw//handle/246246/271992在微胞電泳分離酚類化合物時,界面活性劑十二烷基硫酸鈉(Sodium dodecyl sulfate, SDS)的添加對於酚類分離具有重要的地位。然而,SDS為低揮發性鹽類,對負離子電噴灑有嚴重訊號抑制,且電噴灑時會因為結晶產生而造成噴頭堵塞及噴灑不穩定。本研究將SDS置換為揮發性較佳的十二烷基硫酸銨(Ammonium dodecyl sulfate, ADS),可以避免電灑噴頭堵塞的問題,並搭配壓力輔助雙槽式介面,此介面結合壓力與電場作用力克服鹽類進入質譜造成訊號抑制情形。 介面的組成包括一公分的PVA毛細銜接管連接兩個液體接合槽,一為液體接合電噴灑介面之液體槽,另一液體槽則用於銜接毛細電泳之分離管,銜接毛細電泳分離管之液體槽利用高分子管塞住形成密閉腔體,利用針式幫浦於液體槽加壓。使用PVA毛細銜接管可讓電滲流趨近於零,分析物與ADS只受到電場及側管壓力流的影響,此時由針式幫浦加壓導入80 % 異丙醇可穩定負模式噴灑亦能達到將分析物和ADS拆解,於銜接管施加正電壓使其電場為 +2600 V/cm,使帶負電的ADS停留在後方的液體槽中。將側管有機相pH值調至3,使電泳淌度較小的分析物可隨壓力流推動進到質譜端偵測。介面成功將分析物與ADS作區別,提升分析物在電灑質譜的訊號。Phenols widely used in plastics industry but they were major pollutants when entering the environment. Sodium dodecyl sulfate (SDS) was required for the analysis of phenols by micellar electrokinetic chromatography (MEKC); however, SDS would cause crystals to block the spray tip and also suppress the analyte signals during ionization process in mass interface. In this study, the replacement of SDS by ADS (ammonium dodecyl sulfate) could avoid crystals on the spray tip, and a hydrodynamic flow assisted double junction interface was utilized to alleviate ion suppression from micelles in MEKC-ESI-MS. The transfer column coated with polyvinyl alcohol (PVA) in the interface could decrease the electroosmotic flow (EOF) significantly; therefore, the EOF could be ignored. By introducing organic solvent, the micelles would be collapsed, the ADS would be retained by applying electric field of transfer column, and the analytes would keep moving forward into ESI-MS interface via transfer column by hydrodynamic flow. Consequently, the problem of signal suppression by ADS was alleviated successfully.2895048 bytesapplication/pdf論文公開時間: 2020/8/6論文使用權限: 同意有償授權(權利金給回饋學校)毛細電泳電灑法質譜,壓力輔助雙槽式毛細電泳介面酚類化合物訊號抑制十二烷基硫酸銨MEKC-ESI-MShydrodynamic flow assisted double junction interfaceion suppressionphenolsammonium dodecyl sulfate (ADS)壓力輔助雙槽式毛細管電泳/質譜介面分析酚類化合物訊號改善之研究The Development of Hydrodynamic Flow Assisted Double Junction Interface for Signal Improvement in CE-MS using Negatively Charged Nonvolatile Additivesthesishttp://ntur.lib.ntu.edu.tw/bitstream/246246/271992/1/ntu-104-R02223135-1.pdf