DEVELOPMENT OF A GAS-CHROMATOGRAPHY MASS-SPECTROMETRY METHOD FOR THE ANALYSIS OF AMINOGLYCOSIDE ANTIBIOTICS USING EXPERIMENTAL-DESIGN FOR THE OPTIMIZATION OF THE DERIVATIZATION REACTIONS
M. Preu et al., DEVELOPMENT OF A GAS-CHROMATOGRAPHY MASS-SPECTROMETRY METHOD FOR THE ANALYSIS OF AMINOGLYCOSIDE ANTIBIOTICS USING EXPERIMENTAL-DESIGN FOR THE OPTIMIZATION OF THE DERIVATIZATION REACTIONS, Journal of chromatography, 818(1), 1998, pp. 95-108
Citations number
20
Categorie Soggetti
Chemistry Analytical","Biochemical Research Methods
A packed column GC-electron-capture detection method for the analysis
of the aminoglycoside antibiotics kanamycin and gentamicin was adapted
to capillary GC-MS. The analytes were derivatised using a two-step pr
ocedure involving trimethylsilylation of the hydroxyl groups with trim
ethylsilylimidazole and acylation of the amino groups with heptafluoro
butyrylimidazole. Electron impact mass spectra of the resulting deriva
tives of kanamycin A and gentamicins C-1, C-1a and C-2 are given and i
nterpreted. The derivatisation procedure was optimised using experimen
tal design. This chemometrical approach considers main effects as well
as interactions of the influential parameters, thus conducting a more
thorough investigation of the method than the common step-by-step app
roach. Optimisation using fractional factorial and Box Behnken Designs
produced a derivatisation method featuring better yield than previous
ly published methods while in many cases requiring less reagents and s
horter reaction times. (C) 1998 Elsevier Science B.V. All rights reser
ved.