title: Validated chiral separation of M9, a Mannich ketone compound, by chiral ligand-exchange chromatography.
abstract: Enantioseparation of the Mannich ketone M9, a potential antifungal compound, was examined using chiral ligand-exchange chromatography. The chiral mobile phase contained complexes of Cu(II) with the optically active selector L-aspartame (APM) and the organic modifier methanol. The separation was optimized with respect to the concentration of the Cu(II)-(L-APM) complexes, pH of mobile phase, methanol content, and column temperature. A baseline separation (R(s) = 3.08) was achieved for enantiomers of M9 under optimal conditions, and the analysis was accomplished in eleven minutes. The developed method was extensively validated. The sample stability, linearity, precision (method repeatability and intermediate precision) and accuracy, and the limits of detection and quantification of the developed method were studied. The proposed method was shown to be accurate and suitable for the quantitative determination of each enantiomer of M9.
authors.affiliation: School of Pharmacy, Shenyang Pharmaceutical University, #103 Wenhua Road, Shenyang 110016, China.
authors.forename: Yujin
authors.initials: Y
authors.lastname: Bi
authors.forename: Jing
authors.initials: J
authors.lastname: Yang
authors.forename: Xiumei
authors.initials: X
authors.lastname: Lu
authors.forename: Taili
authors.initials: T
authors.lastname: Shao
authors.forename: Jinhua
authors.initials: J
authors.lastname: Dong
authors.forename: Famei
authors.initials: F
authors.lastname: Li
mesh_terms: D000935:Antifungal Agents / Q000494:pharmacology; D001218:Aspartame / Q000032:analysis; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002845:Chromatography / Q000379:methods*; D003300:Copper / Q000737:chemistry; D000431:Ethanol / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D007659:Ketones / Q000737:chemistry*; D008024:Ligands; D000432:Methanol / Q000737:chemistry; D008956:Models, Chemical; D015203:Reproducibility of Results; D013696:Temperature; D013997:Time Factors
chemical_list: D000935:Antifungal Agents; D007659:Ketones; D008024:Ligands; D000431:Ethanol; D003300:Copper; D000432:Methanol; D001218:Aspartame