title: Identification of novel circulating coffee metabolites in human plasma by liquid chromatography-mass spectrometry.
abstract: This study reports a liquid chromatography-mass spectrometry method for the detection of polyphenol-derived metabolites in human plasma without enzymatic treatment after coffee consumption. Separation of available standards was achieved by reversed-phase ultra performance liquid chromatography and detection was performed by high resolution mass spectrometry in negative electrospray ionization mode. This analytical method was then applied for the identification and relative quantification of circulating coffee metabolites. A total of 34 coffee metabolites (mainly reduced, sulfated and methylated forms of caffeic acid, coumaric acid, caffeoylquinic acid and caffeoylquinic acid lactone) were identified based on mass accuracy (<4 ppm for most metabolites), specific fragmentation pattern and co-chromatography (when standard available). Among them, 19 circulating coffee metabolites were identified for the first time in human plasma such as feruloylquinic acid lactone, sulfated and glucuronidated forms of feruloylquinic acid lactone and sulfated forms of coumaric acid. Phenolic acid derivatives such as dihydroferulic acid, dihydroferulic acid 4'-O-sulfate, caffeic acid 3'-O-sulfate, dimethoxycinnamic acid, dihydrocaffeic acid and coumaric acid O-sulfate appeared to be the main metabolites circulating in human plasma after coffee consumption. The described method is a sensitive and reliable approach for the identification of coffee metabolites in biological fluids. In future, this analytical method will give more confidence in compound identification to provide a more comprehensive assessment of coffee polyphenol bioavailability studies in humans.
authors.affiliation: Metabolomics & Biomarkers Group, Nestlé Research Center, Nestec Ltd., Vers-chez-les-Blanc, 1000 Lausanne, Switzerland. Karine.Redeuil@rdls.nestle.com
authors.forename: Karine
authors.initials: K
authors.lastname: Redeuil
authors.forename: Candice
authors.initials: C
authors.lastname: Smarrito-Menozzi
authors.forename: Philippe
authors.initials: P
authors.lastname: Guy
authors.forename: Serge
authors.initials: S
authors.lastname: Rezzi
authors.forename: Fabiola
authors.initials: F
authors.lastname: Dionisi
authors.forename: Gary
authors.initials: G
authors.lastname: Williamson
authors.forename: Kornél
authors.initials: K
authors.lastname: Nagy
authors.forename: Mathieu
authors.initials: M
authors.lastname: Renouf
mesh_terms: D000328:Adult; D001682:Biological Availability; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002934:Cinnamates / Q000097:blood* / Q000378:metabolism; D003069:Coffee / Q000378:metabolism*; D005260:Female; D020719:Glucuronides / Q000097:blood / Q000378:metabolism; D006801:Humans; D062385:Hydroxybenzoates / Q000097:blood* / Q000378:metabolism; D008297:Male; D011801:Quinic Acid / Q000031:analogs & derivatives* / Q000097:blood / Q000378:metabolism; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D002934:Cinnamates; D003069:Coffee; D020719:Glucuronides; D062385:Hydroxybenzoates; C472707:caffeoylquinic acid; D011801:Quinic Acid