title: Chiral separation of MDL 73,005EF enantiomers using an alpha 1-acid glycoprotein column.
abstract: The enantiomeric separation of MDL 73,005EF (racemic mixture of two enantiomers) has been accomplished using a Chiral AGP (alpha 1-acid glycoprotein) column. The enantiomers are baseline resolved with a runtime of less than 10 min. This separation is used to quantitate the enantiomers present in bulk drug samples, tabletted formulations, and drug used in pharmacological and toxicological studies. Variables found to have an effect on the enantiomeric separation were studied and include: mobile phase ionic strength, type and concentration of organic modifier added to the mobile phase, mobile phase, mobile phase pH, column temperature and the amount of analyte injected. The enantiomeric separation was optimized on the Chiral AGP column based on the effects that each variable had on the separation. Calibration curves for a standard were linear over a range of 0.24 to 61.2 micrograms/g with a correlation coefficient of better than 0.999. A detection limit of 0.012 micrograms/g and a quantitation limit of 0.24 micrograms/g were also found.
authors.affiliation: Pharmaceutical and Analytical Sciences, Marion Merrell Dow Inc., Kansas City, MO 64134, USA.
authors.forename: B M
authors.initials: BM
authors.lastname: Bunton
authors.forename: T A
authors.initials: TA
authors.lastname: Walker
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004147:Dioxins / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D009961:Orosomucoid / Q000737:chemistry*; D009994:Osmolar Concentration; D017366:Serotonin Receptor Agonists / Q000032:analysis*; D013056:Spectrophotometry, Ultraviolet; D013141:Spiro Compounds / Q000032:analysis*; D013237:Stereoisomerism; D013696:Temperature
chemical_list: D004147:Dioxins; D009961:Orosomucoid; D017366:Serotonin Receptor Agonists; D013141:Spiro Compounds; C063249:binospirone mesylate