Abstract
Four dichloro- s-triazine (DCT) and five monochloro-s-triazine (MCT) chiral derivatizing reagents (CDRs) were synthesized by incorporating amino acid amide moieties as chiral auxiliaries in trichloro- s-triazine and its 6-methoxy derivative, respectively. Another MCT reagent was synthesized by substitution of two chlorine atoms with two different amino acid amides in trichloro- s-triazine. These reagents were used for synthesis of diastereomers of ( R,S)-baclofen under microwave irradiation ( i.e. 60 s at 85% power using DCT reagents and 90 s at 85% power using MCT reagents). The diastereomers were separated on a reversed-phase C18 column using mixtures of methanol with aqueous trifluoroacetic acid (TFA) with UV detection at 230 nm. The separation behavior in terms of retention times and resolutions obtained for the two sets of diastereomers prepared with DCT and MCT reagents were compared among themselves and among the two groups. Longer retention times and better resolutions were observed with DCT reagents as compared to MCT reagents. The calibration curves were linear for both ( R)- and ( S)-baclofen in the concentration range 50-500 μg/ml. The average regression was 0.999 for both ( R)- and ( S)-baclofen. The RSD for ( R)-baclofen was 0.40-0.86% for intra-day precision and 0.60-1.40% for inter-day precision and these values for ( S)-baclofen were 0.52-0.75% and 0.64-1.32%, respectively. The recovery was 97.2-98.9% for ( R)- and 97.0-98.9% for ( S)-baclofen. The limit of detection was 1.63ng/ml and 1.52ng/ml for ( R)- and ( S)-baclofen, respectively.
Published Version
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Disclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.