Determination of aminoglutethimide enantiomers in pharmaceutical formulations by capillary electrophoresis using methylated-beta-cyclodextrin as a chiral selector and computational calculation for their respective inclusion complexes.
A capillary electrophoretic method for the separation of the aminoglutethimide (AGT) enantiomers using methylated-beta-cyclodextrin (M-beta-CD) as chiral selector is described. Several parameters affecting the separation were studied, including the type and concentration of chiral selector, buffer pH, voltage and temperature. Good chiral separation of the racemic mixture was achieved in less than 9 min with resolution factor Rs=2.1, using a fused-silica capillary and a background electrolyte (BGE) of tris-phosphate buffer solution (50 mmol L(-1), pH 3.0) containing 30 mgm L(-1) of M-beta-CD. The separation was carried out in normal polarity mode at 25 degrees C, 16 kV and using hydrostatic injection. Acceptable validation criteria for selectivity, linearity, precision, and accuracy/recovery were included. The proposed method was successfully applied to the assay of AGT enantiomers in pharmaceutical formulations. The computational calculations for the inclusion complexes of the R- and S-AGT-M-beta-CD rationalized the reasons for the different migration times between the AGT enantiomers.
Elbashir
Abdalla A
AA
School of Chemical Sciences, Universiti Sains Malaysia, Penang 11800, Malaysia.
Suliman
Fakhr Eldin O
FE
Saad
Bahruddin
B
Aboul-Enein
Hassan Y
HY
D000616:Aminoglutethimide / Q000032:analysis*; D002626:Chemistry, Pharmaceutical / Q000379:methods*; D019075:Electrophoresis, Capillary / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D008956:Models, Chemical; D015394:Molecular Structure; D004364:Pharmaceutical Preparations / Q000032:analysis*; D015203:Reproducibility of Results; D013237:Stereoisomerism; D013696:Temperature; D013997:Time Factors; D047392:beta-Cyclodextrins / Q000032:analysis*
D004364:Pharmaceutical Preparations; D047392:beta-Cyclodextrins; D000616:Aminoglutethimide; C031215:betadex