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Reference type: Journal
Authors: Morante-Zarcero S, Sierra I
Article Title: Comparative HPLC methods for β-blockers separation using different types of chiral stationary phases in normal phase and polar organic phase elution modes. Analysis of propranolol enantiomers in natural waters.
Publication date: 2012
Journal: Journal of Pharmaceutical and Biomedical Analysis
Volume: 62
Issue: (1)
Page numbers: 33-41.
DOI: 10.1016/j.jpba.2011.12.029
Alternative URL: http://www.sciencedirect.com/science/article/pii/S0731708511007369

Abstract: The enantioselectivities of β-blockers (propranolol, metoprolol, atenolol and pindolol) on four different types of chiral stationary phases (CSPs): Chiralpak AD-H, Lux Cellulose-1, Chirobiotic T and Sumichiral OA-4900 were compared using polar organic (PO) elution mode and normal phase (NP) elution mode. Method optimizations were demonstrated by modifying parameters such as organic modifier composition (ethanol, 2-propanol and acetonitrile) and basic mobile phase additives (triethylamine, diethylamine, ethanolamine, and buthylamine). In normal phase elution mode with Lux Cellulose-1, the four pairs of enantiomers can be separated in the same run in gradient elution mode. Additionally, a simple chiral HPLC-DAD method using a newly commercialized polysaccharide-based CSP by Phenomenex (Lux Cellulose-1) in NP elution mode for enantioselective determination of propranolol in water samples by highly selective molecularly imprinted polymers extraction was validated. The optimized conditions were a mobile phase composed by n-hexane/ethanol/DEA (70/30/0.3, v/v/v) at a flow rate of 1.0 mL min-1 and 25 °C. The method is selective, precise and accurate and was found to be linear in the range of 0.125 - 50 μg mL-1 (R2 > 0.999) with a method detection limit (MLD) of 0.4 μg mL-1 for both enantiomers. Recoveries achieved with both enantiomers ranged from 97 to 109%
Template and target information: β-blockers, propranolol
Author keywords: β-Blockers, chiral stationary phase, Natural water samples, Selective molecularly imprinted polymers extraction


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