Efficient molecularly imprinted polymer as a pipette-tip solid-phase sorbent for determination of carvedilol enantiomers in human urine.

Autor: da Silva ATM; Departamento de Ciências Naturais, Universidade Federal de São João del-Rei (UFSJ), Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil., de Oliveira HL; Departamento de Ciências Naturais, Universidade Federal de São João del-Rei (UFSJ), Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil., Silva CF; Departamento de Ciências Naturais, Universidade Federal de São João del-Rei (UFSJ), Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil., Fonseca MC; Departamento de Ciências Naturais, Universidade Federal de São João del-Rei (UFSJ), Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil., Pereira TFD; Departamento de Ciências Naturais, Universidade Federal de São João del-Rei (UFSJ), Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil., Nascimento CS Jr; Departamento de Ciências Naturais, Universidade Federal de São João del-Rei (UFSJ), Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil., de Figueiredo EC; Faculdade de Ciências Farmacêuticas, Universidade Federal de Alfenas (UNIFAL-MG), Rua Gabriel Monteiro da Silva, 700, Centro, 37130-000, Alfenas, MG, Brazil., Borges KB; Departamento de Ciências Naturais, Universidade Federal de São João del-Rei (UFSJ), Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil. Electronic address: keyller@ufsj.edu.br.
Jazyk: angličtina
Zdroj: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences [J Chromatogr B Analyt Technol Biomed Life Sci] 2017 Sep 01; Vol. 1061-1062, pp. 399-410. Date of Electronic Publication: 2017 Aug 01.
DOI: 10.1016/j.jchromb.2017.07.056
Abstrakt: In this work, an efficient pipette tip based on molecularly imprinted polymers solid-phase extraction (PT-MIP-SPE) method was developed for carvedilol (CAR) analysis. This compound is available in clinical practice as a racemic mixture, in which (-)-(S)-CAR is a β- and α 1 -adrenergic antagonist, while (+)-(R)-CAR only acts as an α 1 -adrenergic antagonist. Enantioseparation of CAR presented satisfactory retention times (5.85 and 14.84min), acceptable theoretical plates (N=2048 and 2018) and good resolution (Rs=9.27). The separation was performed using a Chiralpak ® IA column (100mm×4.6mm, 3μm), a mixture of methanol:ethanol:water (64:15:21, v/v/v) plus 0.3% diethylamine as mobile phase, temperature of 35°C and flow rate of 1.5mLmin -1 . After density functional theory calculations based on prepolymerization complexes, the best protocol for the MIP synthesis was chosen. Then, some parameters that affect the PT-MIP-SPE technique were investigated. After optimization, the best conditions were 300μL of water as washing solvent, 500μL of acetonitrile:acetic acid (7:3, v/v) as eluting solvent, 20mg of MIP, 500μL of urine sample (pH 12.5) and no addition of NaCl. Recoveries±relative standard deviation (RSD%) for (+)-(R)-CAR and (-)-(S)-CAR were 101.9±4.8% and 104.6±2.1%, respectively. The method was linear over the concentration range from 20 to 1280ngmL -1 for each enantiomer, with correlation coefficients larger than 0.99 for both enantiomers. The method was applied successfully in a preliminary study of urinary excretion after administration of CAR racemate to a healthy volunteer.
(Copyright © 2017 Elsevier B.V. All rights reserved.)
Databáze: MEDLINE
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