title: Optimized separation of beta-blockers with multiple chiral centers using capillary electrochromatography-mass spectrometry.
abstract: This work focuses on the simultaneous analysis of beta-blockers with multiple stereogenic centers using capillary electrochromatography-mass spectrometry (CEC-MS) with a vancomycin stationary phase. The critical mobile phase variables (composition of organic solvents, acid/base ratios) as well as column temperature and electric field strength, effecting enantioresolution and analysis time were first optimized sequentially. Next, to achieve global optimum a multivariate D-optimal design was used. Although multivariate approach did not improve enantioresolution any further, analysis time was significantly reduced. Under optimum CEC-MS conditions, all stereoisomers were resolved with resolution in the range 1.0-3.1 in less than 60 min with an average signal-to-noise (S/N) greater than 1000. The developed CEC-MS method has the potential to emerge as a screening method for analysis of multiple chiral compounds using a single protocol using the same column and mobile phase conditions, thus reducing the operation time and cost.
authors.affiliation: Department of Chemistry, Center of Biotechnology and Drug Design, Georgia State University, Atlanta, GA 30303, USA.
authors.forename: William
authors.initials: W
authors.lastname: Bragg
authors.forename: Dean
authors.initials: D
authors.lastname: Norton
authors.forename: Shahab A
authors.initials: SA
authors.lastname: Shamsi
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000302:isolation & purification*; D053801:Capillary Electrochromatography / Q000379:methods*; D007741:Labetalol / Q000302:isolation & purification*; D015999:Multivariate Analysis; D009248:Nadolol / Q000302:isolation & purification*; D012997:Solvents; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013237:Stereoisomerism; D013696:Temperature
chemical_list: D000319:Adrenergic beta-Antagonists; D012997:Solvents; D009248:Nadolol; D007741:Labetalol