title: Preconcentration of β-blockers using functionalized ordered mesoporous silica as sorbent for SPE and their determination in waters by chiral CE.
abstract: A method for simultaneous separation and determination of four enantiomeric pairs of β-blockers in waters by chiral CE has been developed. Off-line SPE was employed using functionalized ordered mesoporous silica as sorbent. Separation by CE was achieved using a BGE composed by methylated-β-CD (1.25% w/v) dissolved in a 50 mM phosphate buffer (pH 2.5) and 30°C, with good chiral resolution for all enantiomers. Mesoporous silica functionalized with octadecyl groups (denoted SBA15-C18) was prepared by a postsynthesis method and applied for the preconcentration of atenolol, propranolol, metoprolol, and pindolol enantiomers in waters by off-line SPE. Under optimized conditions, a preconcentration factor of 300 was achieved, employing 100 mg of SBA15-C18 as sorbent, with recoveries between 96 and 105% in tap water and good repeatability (% RSD = 7-11%, n = 6). Commercial C18 amorphous silica (ExtraBondRC18) was also tested as sorbent for SPE, but results revealed better extraction capacity with higher recoveries for the SBA15-C18 material. The analytical characteristics of the off-line SPE-chiral CE method were evaluated, showing good precision, linearity, and accuracy with method quantification limits between 5.3 and 13.7 μg/L for all enantiomers. The SBA15-C18 material allowed the extraction of four enantiomeric pairs of β-blockers spiked in tap water, river water, and ground water with recoveries between 58 and 105%.
authors.affiliation: Departamento de Tecnología Química y Energética, Tecnología Química y Ambiental, Tecnología Mecánica y Química Analítica, ESCET, URJC, Móstoles, Spain.
authors.forename: Mariana
authors.initials: M
authors.lastname: Silva
authors.affiliation: Departamento de Tecnología Química y Energética, Tecnología Química y Ambiental, Tecnología Mecánica y Química Analítica, ESCET, URJC, Móstoles, Spain.
authors.forename: Sonia
authors.initials: S
authors.lastname: Morante-Zarcero
authors.affiliation: Departamento de Tecnología Química y Energética, Tecnología Química y Ambiental, Tecnología Mecánica y Química Analítica, ESCET, URJC, Móstoles, Spain.
authors.forename: Damián
authors.initials: D
authors.lastname: Pérez-Quintanilla
authors.affiliation: Departamento de Química Analítica, Química Física e Ingeniería Química, Facultad de Biología, Ciencias Ambientales y Química, Universidad de Alcalá, Alcalá de Henares, Spain.
authors.forename: María Luisa
authors.initials: ML
authors.lastname: Marina
authors.affiliation: Departamento de Tecnología Química y Energética, Tecnología Química y Ambiental, Tecnología Mecánica y Química Analítica, ESCET, URJC, Móstoles, Spain.
authors.forename: Isabel
authors.identifier: 0000-0003-2091-6772
authors.initials: I
authors.lastname: Sierra
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000032:analysis* / Q000302:isolation & purification; D019075:Electrophoresis, Capillary / Q000379:methods*; D057230:Limit of Detection; D016014:Linear Models; D016062:Porosity; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D000319:Adrenergic beta-Antagonists; D014874:Water Pollutants, Chemical; D012822:Silicon Dioxide
keywords: Chiral capillary electrophoresis; Ordered mesoporous silica; Solid-phase extraction; Water analysis; β-Blockers