Solid phase extraction (SPE) methodology has been evaluated as a cleanup strategy prior to the analysis of phenolic metabolites in fecal samples by UPLC–DAD–ESI–TQ MS. Among the sorbents tested, Oasis® HLB led to the higher phenolic standard recoveries. Sample acidification (0.4 M HCl, final concentration) before SPE considerably improved standard recoveries. Values of the process efficiency (CSPE/CWithout SPE) for a standard solution containing gallic acid, protocatechuic acid, caffeic acid, benzoic acid, 3-phenylpropionic acid, (+)-catechin, (−)-epicatechin, procyanidin B2, and 4-hydroxybenzoic 2,3,5,6 d4 acid were acceptable (>90 %) for all compounds, except for procyanidin B2 (26 %). The developed SPE methodology was applied to fecal samples of individuals subjected to a wine intervention study. Phenolic metabolites, including intermediate metabolites (phenyl-γ-valerolactones and phenylvaleric acid derivatives) and end products (simple phenols, hydroxyphenylpropionic, hydroxyphenylacetic, hydroxycinnamic, and hydroxybenzoic acids) were identified. Most of the compounds (n = 14) exhibited values of process efficiency between 85 and 115 %. Although some compounds (n = 4) showed process efficiency>115 %, there was a group of metabolites (4-O-methylgallic acid, syringic acid, and 4-hydroxy-5-(3′,4′-dihydroxyphenyl)-valeric acid) whose process efficiency was <85 %, which represented a serious limitation and made us to discard SPE as a preparative technique for the analysis of these phenolic metabolites. Finally, the paper reports the concentrations of phenolic metabolites in a randomized set of human fecal samples from healthy volunteers (n = 15) without any previous SPE application. Large inter-individual variability was observed, which was attributed to differences in human gut microbiota composition.
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Authors are grateful to Dr. Rosa del Campo and her group in the Ramón y Cajal Hospital (Madrid, Spain) for providing the feces samples and to Waters (Milford, MA, USA) and Agilent Technologies (Waldbronn, Germany) for providing the cartridges. IMG acknowledges MINECO for her FPI pre-doctorate grant, and FSP and AJG thank CSIC for their respective research contracts. This work has been funded by the Spanish Ministry of Economy and Competitiveness (AGL2009-13361-C02-01, AGL2010-17499, and Consolider Ingenio 2010 FUN-C-FOOD Projects).
Conflicts of Interest
Irene Muñoz-González declares that she has no conflict of interest. Fernando Sánchez-Patán declares that he has no conflict of interest. Ana Jiménez-Girón declares that she has no conflict of interest. Carolina Cueva declares that she has no conflict of interest. María Monagas declares that she has no conflict of interest. Pedro J. Martín-Álvarez declares that he has no conflict of interest. M. Victoria Moreno-Arribas declares that she has no conflict of interest. Begoña Bartolomé declares that she has no conflict of interest.
Compliance with Ethics Requirements
All procedures followed were in accordance with the ethical standards of the Ethics Committee of Clinical Investigation of the CSIC (Spain). Informed consent was obtained from all patients who are included in the study.
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Muñoz-González, I., Sánchez-Patán, F., Jiménez-Girón, A. et al. Evaluation of SPE as Preparative Technique for the Analysis of Phenolic Metabolites in Human Feces. Food Anal. Methods 7, 844–853 (2014). https://doi.org/10.1007/s12161-013-9690-9