Chiral resolution of melatoninergic ligands by EKC using highly sulfated CDs.
EKC methods for the enantiomeric resolutions of melatoninergic ligands were developed using anionic CDs (highly S-alpha-CD, highly S-beta-CD, and highly S-gamma-CD) as chiral selectors at acidic pH 2.5. The optimization of the various operational parameters (nature and concentration of the CD, phosphate buffer concentration, addition of organic modifiers in the BGE, and temperature) allows baseline enantioresolutions (superior to 2) in short analysis times (inferior to 7 min) for all studied analytes. Some analytical characteristics of the optimal method were then studied for each analyte: repeatability, linearity, and LOD and LOQ. Lastly, determination of the apparent binding constants for the 18 complexes formed between the six analytes and the three CDs led us to rationalize the complexation mechanisms.
Lipka
Emmanuelle
E
Laboratoire de Chimie Analytique, EA 4034, Faculté des Sciences Pharmaceutiques et Biologiques, Université de Lille 2- BP 83 - 3, Lille, France.
Danel
Cécile
C
Orhan
Hervé
H
Bonte
Jean-Paul
JP
Vaccher
Claude
C
D002021:Buffers; D020374:Chromatography, Micellar Electrokinetic Capillary / Q000379:methods*; D003505:Cyclodextrins / Q000737:chemistry*; D006863:Hydrogen-Ion Concentration; D007202:Indicators and Reagents; D008024:Ligands; D008550:Melatonin / Q000737:chemistry* / Q000302:isolation & purification / Q000378:metabolism*; D015394:Molecular Structure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013237:Stereoisomerism; D013463:Sulfuric Acid Esters / Q000737:chemistry; D013764:Tetrahydronaphthalenes / Q000737:chemistry* / Q000302:isolation & purification / Q000378:metabolism*; D047392:beta-Cyclodextrins / Q000737:chemistry
D002021:Buffers; D003505:Cyclodextrins; D007202:Indicators and Reagents; D008024:Ligands; D013463:Sulfuric Acid Esters; D013764:Tetrahydronaphthalenes; D047392:beta-Cyclodextrins; D008550:Melatonin