Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
5135646 | Journal of Chromatography A | 2016 | 27 Pages |
Abstract
For the first time, a fully automatized micellar electrokinetic chromatography-mass spectrometry (MEKC-MS) method with in-capillary derivatization was developed for the chiral analysis of d- and l-amino acids using (â)-1-(9-fluorenyl) ethyl chloroformate (FLEC) as labeling reagent. The derivatization procedure was optimized using an experimental design approach leading to the following conditions: sample and FLEC plugs in a 2:1 ratio (15Â s, 30Â mbar: 7.5Â s, 30Â mbar) followed by 15Â min of mixing using a voltage of 0.1Â kV. The formed diastereomers were then separated using a background electrolyte (BGE) consisting of 150Â mM ammonium perfluorooctanoate (APFO) (pHÂ =Â 9.5) and detected by mass spectrometry (MS). Complete chiral resolution was obtained for 8 amino acids, while partial separation was achieved for 6 other amino acid pairs. The method showed good reproducibility and linearity in the low micromolar concentration range. The applicability of the method to biological samples was tested by analyzing artificial cerebrospinal fluid (aCSF) samples.
Related Topics
Physical Sciences and Engineering
Chemistry
Analytical Chemistry
Authors
Radu-Cristian Moldovan, Ede Bodoki, Timea Kacsó, Anne-Catherine Servais, Jacques Crommen, Radu Oprean, Marianne Fillet,