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Enantiomeric separation by using nano‐liquid chromatography with on‐column focusing
Author(s) -
D'Orazio Giovanni,
Fanali Salvatore
Publication year - 2008
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200800114
Subject(s) - chromatography , chemistry , enantiomer , oxprenolol , alprenolol , calibration curve , analytical chemistry (journal) , atenolol , high performance liquid chromatography , detection limit , propranolol , stereochemistry , medicine , biochemistry , receptor , blood pressure , radiology
The present study shows a new nano‐liquid chromatographic method for β‐blocker enantiomers' separation. This method consists of using a capillary column packed with silica particles which were chemically modified with vancomycin. On‐column focusing allowed to inject relatively high sample volumes (1500 nL) increasing method sensitivity. The studied racemic compounds, namely atenolol, propranolol, oxprenolol, and metoprolol were dissolved in methanol and injected for chromatographic separation. The effect of injected sample volume was studied in the range of 50–2100 nL. Peak height of the two alprenolol enantiomers increased linearly up to 1500 nL. This volume was injected for validation and sample analysis. Under optimal experimental conditions, LODs and LOQs (LOD and LOQ for each alprenolol enantiomers) were 9.0 and 15.6 ng/mL, respectively. Calibration curves were linear in the studied range (9–250 ng/mL). The optimized method was applied to the analysis of a human plasma sample spiked with racemic alprenolol.