Environmental chiral analysis of beta-blockers: evaluation of different n-alkyl-modified SBA-15 mesoporous silicas as sorbents in solid-phase extraction
Authors
Marina Alegre, María Luisa; Silva, Mariana; Morante Zarcero, Sonia; Pérez Quintanilla, Damián; Sierra , IsabelIdentifiers
Permanent link (URI): http://hdl.handle.net/10017/48329DOI: 10.1071/EN18030
ISSN: 1448-2517
Date
2018-10Affiliation
Universidad de Alcalá. Departamento de Química Analítica, Química Física e Ingeniería QuímicaBibliographic citation
Environmental Chemistry, 2018, v. 15, n. 6, p. 362-371
Keywords
chiral pharmaceutical compounds
environmental water
functionalised ordered mesoporous silica
Project
Comunidad de Mqadrid y programa FEDER (S2013/ABI-3028, AVANSECAL).
info:eu-repo/grantAgreement/MINECO//CTQ2013-48740-P/ES/METODOLOGIAS AVANZADAS PARA ANALISIS QUIRAL MEDIANTE TECNICAS MICROSEPARATIVAS. BUSQUEDA DE BIOMARCADORES EN SISTEMAS ENANTIOSELECTIVOS/
Document type
info:eu-repo/semantics/article
Version
info:eu-repo/semantics/publishedVersion
Rights
Attribution-NonCommercial-ShareAlike 4.0 International (CC BY-NC-SA 4.0)
© CSIRO Publishing
Access rights
info:eu-repo/semantics/openAccess
Abstract
The extraction and preconcentration of chiral beta-blockers in environmental water was evaluated by solidphase extraction (SPE) employing an SBA-15 ordered mesoporous silica functionalised with alkyl chains of different length. The materials were characterised by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption-desorption isotherm measurements and elemental analysis. Important parameters influencing extraction efficiency, including the type and amount of sorbent and the breakthrough volume, were optimised. The results obtained showed that the organic chain length played an important role in the behaviour of these sorbents. Under optimised conditions, using 200 mg SBA-15-C8 as sorbent, a simple analytical method based on off-line SPE coupled to chiral capillary electrophoresis with diode array detection (SPE-chiral CE-DAD) was developed. Method detection and quantification limits were lower than 0.6 and 1.9 mu g L-1 respectively for all enantiomers, with a preconcentration factor of 500-fold. The method was successfully applied to the chiral analysis of atenolol, metoprolol, pindolol and propranolol in river and sewage water samples. Satisfactory recoveries (between 86 +/- 2 and 98 +/- 1 %) and repeatability (relative standard deviation (RSD) < 9 %, n = 3) were obtained. Metoprolol was detected in sewage water at a concentration of 10.7 and 9.9 mu g L-1 and an enantiomeric fraction of 0.52 and 0.48 for the first- and the second-migrating enantiomers respectively. These results emphasise the importance of enantioselective analysis for environmental risk assessment.
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