Enantioseparation of vesamicol in human serum by capillary electrophoresis with solid phase extraction and sulfated-beta-cyclodextrin.
An enantioseparation of racemic vesamicol in human serum by capillary electrophoresis with solid phase extraction and sulfated B-cyclodextrin (S-B-CD) is presented The separation was achieved on an uncoated 72 cm x 50 microm id fused silica capillary maintained at 30 degrees C and + 15 kV applied voltage using a run buffer of 128 micro-B-CD in 50 mM phosphate buffer at pH 5. The detection wavelength was 260 nm. Bond Elut C18 solid phase extraction cartridges were used in the sample preparation of the vesamicol samples from serum. Among the CDs studied, the migration order of the enantiomers was reversed in CM-B-CD compared to S-B-CD. Increases in migration time and differences in time between enantiomers was observed with increasing concentrations of S-B-CD. Baseline separation was achieved in the 2-20 microg/ml range of enantiomer concentration (r > .996). A sample stacking technique was used to improve peak shape and LOD. LODs were 0.5 microg/ml for each enantiomer. Studies of various factors and CE conditions showed the effect of CD type, CD concentration, buffer type, buffer concentration and pH on stability and resolution.
D003505:Cyclodextrins / Q000032:analysis*; D019075:Electrophoresis, Capillary / Q000379:methods; D006801:Humans; D010880:Piperidines / Q000097:blood* / Q000737:chemistry; D013237:Stereoisomerism; D013431:Sulfates / Q000032:analysis*; D047392:beta-Cyclodextrins
D003505:Cyclodextrins; D010880:Piperidines; D013431:Sulfates; D047392:beta-Cyclodextrins; C006189:vesamicol; C031215:betadex