Enantiomeric separation of baclofen by capillary electrophoresis tandem mass spectrometry with sulfobutylether-beta-cyclodextrin as chiral selector in partial filling mode.
Capillary electrophoresis (CE) coupled to tandem mass spectrometry was applied to the chiral separation of baclofen using sulfobutylether-beta-cyclodextrin chiral selector in partial filling counter current mode. On-line UV detection was simultaneously used. Method optimization was performed by studying the effect of cyclodextrin and BGE concentration as well as sheath liquid composition on analyte migration time and enantiomeric resolution. The cyclodextrin showed stereoselective complexation towards baclofen enantiomers, allowing chiral resolution at low concentration. The CE capillary protrusion from the ESI needle relevantly affected the chiral resolution and the analyte migration time. Complete enantiomeric separation was obtained by using 0.25 M formic acid BGE containing 1.75 mM of chiral selector and water/methanol (30:70, v/v) 3% formic acid as sheath liquid. The method exhibited a LOD of 0.1 microg/mL (racemic concentration) in MS3 product ion scan mode of detection and was applied to the analysis of racemic baclofen in pharmaceutical formulations.
Desiderio
Claudia
C
Istituto di Chimica del Riconoscimento Molecolare, Consiglio Nazionale delle Ricerche, L.go F. Vito 1, 00168 Roma, Italy. claudia.desiderio@icrm.cnr.it
Rossetti
Diana Valeria
DV
Perri
Fabio
F
Giardina
Bruno
B
Messana
Irene C
IC
Castagnola
Massimo
M
D001418:Baclofen / Q000302:isolation & purification*; D019075:Electrophoresis, Capillary / Q000295:instrumentation / Q000379:methods*; D005561:Formates / Q000737:chemistry; D004364:Pharmaceutical Preparations / Q000737:chemistry; D012680:Sensitivity and Specificity; D013237:Stereoisomerism; D053719:Tandem Mass Spectrometry / Q000379:methods*; D047392:beta-Cyclodextrins
D005561:Formates; D004364:Pharmaceutical Preparations; D047392:beta-Cyclodextrins; C030544:formic acid; C093196:SBE4-beta-cyclodextrin; D001418:Baclofen