N-Menthoxycarbonylation combined with trimethylsilylation for enantioseparation of beta-blockers by achiral dual-column gas chromatography.
Solvent extractive two-phase menthoxycarbonyl (MnOC) derivatization was combined with trimethylsilyl (TMS) reaction for enantioseparation of beta-blockers by gas chromatography employing achiral DB-5 and DB-17 dual-columns of different polarity. beta-Blockers in alkaline solution were vortex-mixed with menthyl chloroformate present in dichloromethane to be extracted as diastereomeric N-MnOC derivatives. The subsequent O(N)-TMS reaction allowed complete enantioseparations of two beta-blockers and partial separations of five as N-MnOC/O(N)-TMS derivatives in a single analysis. The temperature-programmed retention index sets were characteristic of each derivative, facilitating chiral discrimination of each enantiomer.
Paik
Man-Jeong
MJ
Biometabolite Analysis Laboratory, College of Pharmacy, Sungkyunkwan University, Suwon 440-746, South Korea.
Nguyen
Duc-Toan
DT
Kim
Kyoung-Rae
KR
D000319:Adrenergic beta-Antagonists / Q000737:chemistry* / Q000302:isolation & purification*; D002849:Chromatography, Gas / Q000379:methods*; D005561:Formates / Q000737:chemistry*; D013237:Stereoisomerism; D014297:Trimethylsilyl Compounds / Q000737:chemistry*
D000319:Adrenergic beta-Antagonists; D005561:Formates; D014297:Trimethylsilyl Compounds; C059663:menthyl chloroformate