[Enantiomeric determination of ephedrine derivatives in unregulated drugs using capillary electrophoresis].
Capillary electrophoresis (CE) was applied to enantiomeric separation of chiral ephedrine derivatives (d/l-ephedrine, d/l-methylephedrine, d/l-pseudoephedrine, and d/l-norephedrine) in unregulated drug products. Unregulated drugs, referred to as dietary supplements in U.S.A., have been used legally as tonic agents, but illegal substances such as ephedrine were often detected. Baseline separation of all enantiomers of ephedrine derivatives was achieved using an electrophoretic solution containing heptakis (2,6-di-O-methyl)-beta-cyclodextrin (DM-CD) as a chiral selector. The optimal conditions were established to be: capillary column of fused silica (50 microm i.d. x 56 cm); running buffer of 20 mM DM-CD with 50 mM potassium dihydrogenphosphate background electrolyte, pH 2.6; capillary temperature of 20 degrees C; applied voltage of 30 kV; on-column detection at 195 nm; and injection pressure of 50 mbar x 3 s. Under these conditions, all four pairs of enantiomers were sufficiently resolved, and eight peaks were observed with resolution factors of greater than 1.5. The calibration curves of all enantiomers showed good linearity over the concentration range of 2.5-10 microg/ml (r =0.999). The present method was used in a survey of marketed products. The resultant chiral contents were reported and the analytical data were also compared with those from HPLC. This method is useful in the simple and rapid analysis of ephedrine derivatives in marketed products.
Miyatake
Norie
N
Tama Branch Institute, Tokyo Metropolitan Institute of Public Health, Tachikawa, Japan. Norie_Miyatake@member.metro.tokyo.jp
Miyake
Hirofumi
H
Nagashima
Machiko
M
Takahashi
Misako
M
Yasuda
Kazuo
K
Yasuda
Ichiro
I
D002851:Chromatography, High Pressure Liquid; D003505:Cyclodextrins; D019587:Dietary Supplements / Q000032:analysis*; D019075:Electrophoresis, Capillary / Q000379:methods*; D004809:Ephedrine / Q000031:analogs & derivatives* / Q000302:isolation & purification*; D013287:Illicit Drugs / Q000032:analysis*; D015203:Reproducibility of Results; D013237:Stereoisomerism; D047392:beta-Cyclodextrins
D003505:Cyclodextrins; D013287:Illicit Drugs; D047392:beta-Cyclodextrins; C038119:heptakis(2,6-O-dimethyl)beta-cyclodextrin; D004809:Ephedrine