KMID : 0385520210340010009
|
|
Analytical Science & Technology 2021 Volume.34 No. 1 p.9 ~ p.16
|
|
1H-NMR and HPLC analysis on the chiral discrimination of ¥â-blockers using (S)-2-tert-butyl-2-methyl-1,3-benzodioxole-4-carboxylic acid
|
|
Seo Sang-Hun
Mai Xuan-Lan Le Thi-Anh-Tuyet Kim Kyeong-Ho
|
|
Abstract
|
|
|
In the group of commonly prescribed ¥â-blocker drugs, one of the enantiomers is generally relatively more active than the others. This study aims to develop a technique for the chiral analysis of select ¥â-blockers based on proton nuclear magnetic resonance (1H-NMR) spectrometry. (S)-2-Tert-butyl-2-methyl-1,3-benzodioxole-4- carboxylic acid ((S)-TBMB) was synthesized and utilized as a chiral derivatizing agent. Pure ¥â-blocker enantiomers were isolated from racemates by semi-preparative liquid chromatography prior to derivatization.
The reaction time and concentration of (S)-TBMB were controlled to improve the derivatization procedure. No racemization was found during the analysis. High-performance liquid chromatography (HPLC) analysis was also performed for comparative purposes. High agreement between the NMR and HPLC methods was achieved in the determination of (R)-metoprolol in a standard solution of the (S) isomer.
|
|
KEYWORD
|
|
¥â-blockers, Chiral derivatizing agent, 1H-NMR, HPLC
|
|
FullTexts / Linksout information
|
|
|
|
Listed journal information
|
|
|