부산대학교 도서관

To link to full-text access for this article, visit this link: http://dx.doi.org/10.1016/j.chroma.2005.06.021 Byline: Romain Jacquet, Patrick Favetta, Claire Elfakir, Michel Lafosse Keywords: Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry; High-performance liquid chromatography; Evaporative light scattering detection; Methylated [beta]-cyclodextrins; Degree of substitution Abstract: A new methylated [beta]-cyclodextrin with a low degree of substitution was characterized by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and high-performance liquid chromatography (HPLC) with evaporative light scattering detection. Using [alpha]-cyano-4-hydroxycinnamic acid as the matrix and the thin layer method as the deposition procedure, MALDI-TOF-MS revealed that the mixture was composed of CDs bearing from 2 to 8 methyl groups with an average degree of substitution (DS) of 0.7 (i.e. 0.7 methyl groups per glucopyranose unit). Using a Purospher Star RP-18 endcapped column with acetonitrile-water mobile phase in gradient elution mode, HPLC was employed at analytical scale to obtain a chromatographic fingerprint of the crude mixture and at semi-preparative scale to fractionate it. MALDI-TOF-MS of these fractions revealed that the overall retention of the different derivatives, which depicts their polarity, was mainly driven by the DS and increased with the number of methyl groups on the CD moiety. Author Affiliation: Institut de Chimie Organique et Analytique, UMR CNRS 6005, FR 2708, Universite d'Orleans, UFR Sciences, BP 6759, rue de Chartres, 45067 Orleans Cedex 2, France Article History: Received 17 March 2005; Revised 30 May 2005; Accepted 6 June 2005