毛細管電泳電灑法質譜檢測全氟烷基羧酸類化合物

全氟界面活性劑包括了全氟烷基酸羧類化合物，在此類化合物的檢測上一般會採以液相層析搭配質譜儀的檢測(LC-MS)。然而在本研究中，希望藉由毛細管電泳質譜法(CE-MS)來分析該類化合物。一開始以低流速鞘流電灑界面作為電泳銜接質譜的界面，在醋酸銨系統下討論各個毛細管電泳分離之參數(如pH值、緩衝溶液濃度、有機添加劑)對分離的影響，希望能找到最佳的緩衝溶液組成以達到快速而又靈敏的分析。另一方面，文獻及實驗結果(UV偵測)皆顯示若使用磷酸鹽緩衝溶液時，能得到比醋酸鹽緩衝溶液系統更佳的分離效率。因此若希望保有磷酸鹽在分離上的優點而又不使其影響分析物訊號，在實驗設計上會以液體接合-低流速鞘流界面來克服此問題。實驗中發現必須控制電滲流速度與磷酸陰離子後退的速度，而使得磷酸在整個分析過程中不會被帶往質譜端，進而造成分析物訊號的干擾或抑制。若選擇15mM磷酸銨、pH值8.3 於50% 甲醇水溶液下，磷酸根離子並不會進入質譜端，且可在15分鐘內完成分析。

關鍵字

毛細管電泳；質譜；全氟化合物

並列摘要

Perfluoroalkylcarboxylates and perfluoroalkyksulfonates are popular fluorinated surfactants. Generally, the detection of these compounds was based on LC-MS technique. In this study, we try to use CE-MS as the tool to develop a rapid and sensitive method for the analysis of perfluorocompounds(PFCs). First, the low-flow interface was tested and ammonium acetate was used as the running buffer. Factors which may influence separation efficiency includes pH value, buffer concentration and organic solvents were studied. By varying these factors, we could get a optimized separation condition for PFCs analysis. However, phosphate buffer was reported to give better separation than acetate buffer in CE-UV. Unfortunately, phosphate buffer is shown to cause interference or suppress analyte signal. A liquid junction-low flow CE-MS interface was studied to alleviate these problems. In this design, phosphate buffer was placed in the liquid-junction reservoir. The mobility of EOF and phosphate ions needs to be controlled. At a concentration of 15mM ammonium phosphate in 50% MeOH, pH=8.3, the CE-MS interface demonstrated its utility to prevent phosphate ions entering the MS ionization source.

並列關鍵字

Electrophoresis ； Mass Spectrometry ； Perfluorocarboxylic acids

參考文獻

Med. 1999, 41, 799–806.

3. Giesy, J.P.; Kannan, K. Environ. Sci. Technol. 2002, 36, 147A–152A.

4. Wickbold, R. Angew. Chem. 1954, 66, 173–174.

Anal. Chem. 2001, 73, 2200–2206.

6. Belisle, J.; Hagen, D.F. Anal. Biochem. 1980, 101, 369–376.

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毛細管電泳電灑法質譜檢測全氟烷基羧酸類化合物

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