A Molecularly Imprinted Polymer for Selective Extraction of Phenolic Acids from Human Urine

Studies for monitoring the bioavailability of dietary flavonoid compounds generate great interest. Among them, low-molecular-weight phenolic acids, secondary metabolites present in colonic catabolism and urinary excretion, have been proposed as biomarkers of polyphenol intake. Using 4-hydroxyphenyla...

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Main Authors: Marco Mora-Granados, David González-Gómez, Jin Su Jeong, Alejandrina Gallego-Picó
Format: Article
Language:English
Published: MDPI AG 2021-02-01
Series:Applied Sciences
Subjects:
Online Access:https://www.mdpi.com/2076-3417/11/4/1577
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spelling doaj-a765e129798449f3b457e7bc113f24eb2021-02-10T00:06:02ZengMDPI AGApplied Sciences2076-34172021-02-01111577157710.3390/app11041577A Molecularly Imprinted Polymer for Selective Extraction of Phenolic Acids from Human UrineMarco Mora-Granados0David González-Gómez1Jin Su Jeong2Alejandrina Gallego-Picó3Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), 28040 Madrid, SpainDepartment of Didactic of Experimental Sciences and Mathematics Education, University of Extremadura (UNEX), 10071 Cáceres, SpainDepartment of Didactic of Experimental Sciences and Mathematics Education, University of Extremadura (UNEX), 10071 Cáceres, SpainDepartment of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), 28040 Madrid, SpainStudies for monitoring the bioavailability of dietary flavonoid compounds generate great interest. Among them, low-molecular-weight phenolic acids, secondary metabolites present in colonic catabolism and urinary excretion, have been proposed as biomarkers of polyphenol intake. Using 4-hydroxyphenylacetic acid as a template, a molecularly imprinted polymer (MIP) was synthesized for selective extraction of these hydroxylated metabolites from human urine samples and posterior analysis in an HPLC-DAD-MS system. Polymers were characterized by Scanning electron microscopy (SEM), Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), Brunauer-Emmett-Teller (BET) method, and binding experiments. MIP presents specific recognition ability for template and analogues molecules. This capacity of recognition and the pH dependence of the binding strength was also studied. The method was validated over a concentration range of 0.25–40 mg/L, r<sup>2</sup> > 0.995. In the optimized conditions, the recovery value was 94% with RSD 1.2%. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were 1.22 and 3.69 mg/L, respectively. In our knowledge, it is the first time that this methodology is applied to analyze urinary catabolites of the polyphenol compound and to provide a specific method and simple analysis alternative. The selective extraction of these metabolites improves the application and results obtained by other less sensitive analysis methods than the validation method. It also facilitates the development of new screening methods.https://www.mdpi.com/2076-3417/11/4/1577molecularly imprinted polymerpolyphenol metabolitessolid phase extractionhuman urinephenolic acidsHPLC-DAD-MS
collection DOAJ
language English
format Article
sources DOAJ
author Marco Mora-Granados
David González-Gómez
Jin Su Jeong
Alejandrina Gallego-Picó
spellingShingle Marco Mora-Granados
David González-Gómez
Jin Su Jeong
Alejandrina Gallego-Picó
A Molecularly Imprinted Polymer for Selective Extraction of Phenolic Acids from Human Urine
Applied Sciences
molecularly imprinted polymer
polyphenol metabolites
solid phase extraction
human urine
phenolic acids
HPLC-DAD-MS
author_facet Marco Mora-Granados
David González-Gómez
Jin Su Jeong
Alejandrina Gallego-Picó
author_sort Marco Mora-Granados
title A Molecularly Imprinted Polymer for Selective Extraction of Phenolic Acids from Human Urine
title_short A Molecularly Imprinted Polymer for Selective Extraction of Phenolic Acids from Human Urine
title_full A Molecularly Imprinted Polymer for Selective Extraction of Phenolic Acids from Human Urine
title_fullStr A Molecularly Imprinted Polymer for Selective Extraction of Phenolic Acids from Human Urine
title_full_unstemmed A Molecularly Imprinted Polymer for Selective Extraction of Phenolic Acids from Human Urine
title_sort molecularly imprinted polymer for selective extraction of phenolic acids from human urine
publisher MDPI AG
series Applied Sciences
issn 2076-3417
publishDate 2021-02-01
description Studies for monitoring the bioavailability of dietary flavonoid compounds generate great interest. Among them, low-molecular-weight phenolic acids, secondary metabolites present in colonic catabolism and urinary excretion, have been proposed as biomarkers of polyphenol intake. Using 4-hydroxyphenylacetic acid as a template, a molecularly imprinted polymer (MIP) was synthesized for selective extraction of these hydroxylated metabolites from human urine samples and posterior analysis in an HPLC-DAD-MS system. Polymers were characterized by Scanning electron microscopy (SEM), Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), Brunauer-Emmett-Teller (BET) method, and binding experiments. MIP presents specific recognition ability for template and analogues molecules. This capacity of recognition and the pH dependence of the binding strength was also studied. The method was validated over a concentration range of 0.25–40 mg/L, r<sup>2</sup> > 0.995. In the optimized conditions, the recovery value was 94% with RSD 1.2%. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were 1.22 and 3.69 mg/L, respectively. In our knowledge, it is the first time that this methodology is applied to analyze urinary catabolites of the polyphenol compound and to provide a specific method and simple analysis alternative. The selective extraction of these metabolites improves the application and results obtained by other less sensitive analysis methods than the validation method. It also facilitates the development of new screening methods.
topic molecularly imprinted polymer
polyphenol metabolites
solid phase extraction
human urine
phenolic acids
HPLC-DAD-MS
url https://www.mdpi.com/2076-3417/11/4/1577
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