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Photometric detection of cyclodextrins in liquid chromatography by using iodine generated electrochemically in-situ
Authors:Toshiya?Hiroi  Email author" target="_blank">Jiye?JinEmail author  Toyohide?Takeuchi
Institution:(1) Department of Chemistry, Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan;(2) Department of Chemistry, Faculty of Science, Shinshu University, 3-1-1 Asahi, Matsumoto, Nagano 390-8621, Japan
Abstract:A method has been developed for photometric detection of cyclodextrins (CD) in liquid chromatography using iodine (I2) generated electrochemically in-situ. Iodide ion in the mobile phase was electrochemically oxidized to I2 which was subsequently reacted with I, in an electrochemical flow cell, forming I3. The absorbance of I3 was found to be greatly enhanced when CD were present in the mobile phase. The absorbance enhancement was caused by the change in the mole fraction of I3, because of the inclusion reaction of I3 with CD. On the basis of this phenomenon, CD were detected by means of a photodiode-array UV–visible detector positioned downstream of the electrochemical flow cell. The signals were found to be linearly dependent on CD concentration. Because the formation constants of I3 with CD decrease in the order agr-CD>beta-CD>gamma-CD, agr-CD was most detectable by the method. Detection limits were 1.0 mgrmol L–1 for agr-CD, 65 mgrmol L–1 for monoG1-beta-CD, 100 mgrmol L–1 for beta-CD, and 200 mgrmol L–1 for gamma-CD.
Keywords:Cyclodextrins  Iodine  Inclusion reaction  Electrochemical flow cell  Cyclic voltammetry  Liquid chromatography
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