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Radiosynthesis of 1-(2-[18F]Fluoroethyl)-L-Tryptophan using a One-pot, Two-step Protocol
Published on: September 21, 2021
Semi-preparative enantiomeric separation of ofloxacin by HPLC
Zhili Fang1, Ziyuan Guo, Qing Qin
1Institute of Special Materials/School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China.
Abstract:
A direct semi-preparative high performance liquid chromatography (HPLC) enantioseparation of ofloxacin was performed on chemically immobilized cyclodextrin derivative-mono (6A-azido-6A-deoxy)-per(p-chlorophenyl carbamoylated) β-CD chiral stationary phase. Conditions for semi-preparative separations were established using a 250 × 4.6 mm i.d. column and subsequently extended to a 250 × 10.0 mm i.d. column that enabled separations on a milligram scale. Optimization of the chromatographic conditions (mobile phase and column load) with respect to better efficiency, resolution and peak retention resulted in a system capable of separating up to 304 mg of (-)-(S)-ofloxacin and 56 mg of (+)-(R)-ofloxacin of the racemate over 6 h. The purities of the separated enantiomers were determined by HPLC. Moreover, both separated enantiomers were characterized by mass spectrometry; then, the absolute configuration of the products was clearly confirmed by polarimetry.
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