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Evaluation of SPE as Preparative Technique for the Analysis of Phenolic Metabolites in Human Feces

AuthorsMuñoz-González, Irene ; Sánchez-Patán, Fernando ; Jiménez-Girón, Ana ; Cueva, Carolina ; Monagas Juan, María Josefina ; Martín-Álvarez, Pedro J. ; Moreno-Arribas, M. Victoria ; Bartolomé, Begoña
KeywordsSolid phase extraction
Human feces
Phenolic metabolites
Issue Date2014
CitationFood Analytical Methods 7(4): 844-853 (2014)
AbstractSolid 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. © 2013 Springer Science+Business Media New York.
Identifiersdoi: 10.1007/s12161-013-9690-9
issn: 1936-9751
e-issn: 1936-976X
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