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1.
J Chromatogr A ; 1410: 164-72, 2015 Sep 04.
Artigo em Inglês | MEDLINE | ID: mdl-26256924

RESUMO

A molecularly imprinted polymer (MIP) based methodology is described here for the determination of compounds that belong to the 4-ethylphenol (4EP) metabolic pathway in red wines. To this end, two MIP materials have been developed: a 4EP MIP as a class-selective material to extract phenols that belong to the 4EP metabolic pathway and a coumaric acid (CA) imprinted polymer as a MIP-based stationary phase capable of selectively separating these phenols on HPLC analysis, obtaining clean chromatograms. 4-vinyl pyridine and ethylene glycol dimethacrylate were respectively used as functional monomer and cross-linker for both MIPs. Once polymer compositions were optimised, the 4EP MIP was packed into SPE cartridges for wine sample clean-up and CA MIP was packed into HPLC columns to chromatographically separate the compounds present in the eluates obtained after SPE extraction. The accuracy of the proposed method was tested spiking wine samples with known concentrations of target compounds and subsequently, analytes were quantified by the standard addition method. Registered mean recoveries ranged from 95.2 to 109.2% and RSD values were below 10% in most cases. The described methodology was found to be suitable for the selective extraction and quantification of the compounds that belong to the 4EP metabolic pathway in red wines with minimal matrix effects and could be undoubtedly exploited to monitor 4EP and its precursors in wines.


Assuntos
Metacrilatos/química , Impressão Molecular , Fenóis/metabolismo , Polietilenoglicóis/química , Polivinil/química , Vinho/análise , Cromatografia Líquida de Alta Pressão/métodos , Redes e Vias Metabólicas , Extração em Fase Sólida/métodos
2.
Talanta ; 116: 448-53, 2013 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-24148428

RESUMO

This paper reports the application of a chiral imprinted polymer (CIP)-coated stir bar for the selective extraction of (+)-(S)-citalopram (SCIT) and its main metabolites, (+)-(S)-desmethylcitalopram (SDCIT) and (+)-(S)-didesmethylcitalopram (SDDCIT), from urine samples. The developed device has been demonstrated to be capable of selectively extracting the three target analytes from urine samples without saturating the imprinted sites. A CIP-coated stir bar sorptive extraction procedure (CIP-SBSE) is proposed for the isolation of SCIT, SDCIT and SDDCIT followed by their subsequent analysis using liquid chromatography ion trap mass spectrometry (LC-ITMS). Deuterated SCIT-d6 was used as an internal standard. The method was validated using a standard procedure, which revealed that a quantification of 5 ng mL(-1) was obtained in urine samples and that the accuracy and precision were within the established values while no matrix effect was observed.


Assuntos
Antidepressivos de Segunda Geração/urina , Citalopram/análogos & derivados , Citalopram/urina , Polímeros/química , Extração em Fase Sólida/normas , Adsorção , Cromatografia Líquida , Humanos , Impressão Molecular/métodos , Padrões de Referência , Sensibilidade e Especificidade , Extração em Fase Sólida/métodos , Espectrometria de Massas por Ionização por Electrospray , Estereoisomerismo , Espectrometria de Massas em Tandem
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