https://scholars.lib.ntu.edu.tw/handle/123456789/178186
標題: | 毛細管電層析/電灑法質譜儀之開發與應用 | 作者: | 莊育傑 | 關鍵字: | 毛細管電層析;電灑法;除草劑;capillary electrochromatography;CEC;electrospray ionization;ESI;triazine | 公開日期: | 2004 | 摘要: | 毛細管電層析(capillary electrochromatography , CEC)是結合毛細管電泳與高效能液相層析之特性的分離技術,藉由此特性可分離帶電荷及中性的分析物。以電灑法(electrospray ionization , ESI)質譜儀做為偵測器時,可以由滯留時間與質量做為定性的依據。 在毛細管區帶電泳下,分析市售常見的八種除草劑,卻無法有效的達到分離效果;實驗室曾經使用微胞電動電泳(MEKC),成功的分離這八種除草劑,但是在接上質譜儀分析後,由於緩衝溶液中加入非揮發性的添加劑(介面活性劑SDS),造成在離子化的過程中,添加劑與分析物互相競爭液珠過量電荷而抑制質譜訊號;本實驗的目的在捨去介面活性劑(SDS)的使用,避免SDS對除草劑質譜訊號的抑制,改以開管式毛細管(C8)與填充式毛細管(C18)為分離工具,利用靜相與除草劑間的作用力達到分離的效果;此外,實驗中將緩衝溶液醋酸銨的濃度降低,使醋酸銨對除草劑的抑制現象降到最低。 Capillary electrochromatography (CEC) can be considered to be a hybrid of capillary electrophoresis (CE) and high performance liquid chromatography (HPLC) that has the potential to become a powerful separation tool for the analysis of charge and neutral mixtures. Electrospray ionization (ESI)-MS is the best chromatography detector available for both retention time and mass analysis. The eight commercial triazine cannot be separated effectively by capillary zone electrophoresis (CZE). Thus, in previous work, micellar electrokinetic chromatography (MEKC) has been tried and the method can successfully separate the eight triazine. However, when MEKC couples with MS, the nonvolatile surfactant has been added to the buffer solution NH4OAc. So in the process of ionization, the surfactant and analyte compete the surface charge of droplet with each other. Therefore, the purpose of this experiment is giving up the use of SDS so that the inhibitioin of signal can be avoided. We use ot-CEC and packed-CEC instead, and the efficiency of separation can be achieved by the partition between stationary and mobile phase. Besides, we reduce the concentration of buffer solution NH4OAc and make the inhibition of signal much lower. |
URI: | http://ntur.lib.ntu.edu.tw//handle/246246/51891 | 其他識別: | zh-TW |
顯示於: | 化學系 |
檔案 | 描述 | 大小 | 格式 | |
---|---|---|---|---|
ntu-93-R91223015-1.pdf | 23.31 kB | Adobe PDF | 檢視/開啟 |
在 IR 系統中的文件,除了特別指名其著作權條款之外,均受到著作權保護,並且保留所有的權利。