Dataset Information

GNPS LC-MSn study of human urine samples containing Green Tea breakdown products

ABSTRACT: Abstract: In dietary polyphenol exposure studies, annotation and identification of urinary metabolites present at low (micromolar) concentrations are major obstacles. To determine the biological activity of specific components, it is necessary to have the correct structures and the quantification of the polyphenol-derived conjugates present in the human body. We present a procedure for identification and quantification of metabolites and conjugates excreted in human urine after single bolus intake of black or green tea. A combination of a solid-phase extraction (SPE) preparation step and two high pressure liquid chromatography (HPLC)-based analytical platforms was used, namely, accurate mass fragmentation (HPLC-FTMSn) and mass-guided SPE-trapping of selected compounds for nuclear magnetic resonance spectroscopy (NMR) measurements (HPLC-TOFMS-SPE-NMR). HPLC-FTMSn analysis led to the annotation of 138 urinary metabolites, including 48 valerolactone and valeric acid conjugates. By combining the results from MSn fragmentation with the one-dimensional (1D)-1H NMR spectra of HPLC-TOFMS-SPE-trapped compounds, we elucidated the structures of 36 phenolic conjugates, including the glucuronides of 3?,4?-di- and 3?,4?,5?-trihydroxyphenyl-?-valerolactone, three urolithin glucuronides, and indole-3-acetic acid glucuronide. We also obtained 26 h-quantitative excretion profiles for specific valerolactone conjugates. The combination of the HPLC-FTMSn and HPLC-TOFMS-SPE-NMR platforms results in the efficient identification and quantification of less abundant phenolic conjugates down to nanomoles of trapped amounts of metabolite corresponding to micromolar metabolite concentrations in urine. Sample description: Four healthy male volunteers (24, 25, 28, and 55 years) followed the polyphenol-low diet for 3 days prior to green tea intake. Volunteers consumed 1.5 L of green tea (6 grams of China Bancha Green tea extracted with 1.0 L hot water for 5 minutes). Urine samples were collected in 50 ml tubes until 26 hours after intake - fractions were indicated with letters starting at A. Immediately after collection, the volume of the sample was recorded, and the urine samples were stored at 4 ?C for maximal 24 hours before transferring to -80 ?C.

INSTRUMENT(S): LTQ Orbitrap

ORGANISM(S): Homo Sapiens (ncbitaxon:9606)

SUBMITTER: Justin van der Hooft

PROVIDER: MSV000081878 | GNPS | Wed Jan 03 03:57:00 GMT 2018

REPOSITORIES: GNPS

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Publications

Structural elucidation and quantification of phenolic conjugates present in human urine after tea intake.

van der Hooft Justin J J JJ de Vos Ric C H RC Mihaleva Velitchka V Bino Raoul J RJ Ridder Lars L de Roo Niels N Jacobs Doris M DM van Duynhoven John P M JP Vervoort Jacques J

Analytical chemistry 20120802 16

In dietary polyphenol exposure studies, annotation and identification of urinary metabolites present at low (micromolar) concentrations are major obstacles. To determine the biological activity of specific components, it is necessary to have the correct structures and the quantification of the polyphenol-derived conjugates present in the human body. We present a procedure for identification and quantification of metabolites and conjugates excreted in human urine after single bolus intake of blac ...[more]

PMID: 22827565

Similar Datasets

Project description:Abstract of the study: Advanced analytical approaches consisting of both LC-LTQ-Orbitrap Fourier transformed (FT)-MS and LC-time-of-flight-(TOF)-MS coupled to solid-phase extraction (SPE) NMR were used to obtain more insight into the complex phenolic composition of tea. On the basis of the combined structural information from (i) accurate mass fragmentation spectra, derived by using LC-Orbitrap FTMSn, and (ii) proton NMR spectra, derived after LC-TOFMS triggered SPE trapping of selected compounds, 177 phenolic compounds were annotated. Most of these phenolics were glycosylated and acetylated derivatives of flavan-3-ols and flavonols. Principal component analysis based on the relative abundance of the annotated phenolic compounds in 17 commercially available black, green, and white tea products separated the black teas from the green and white teas, with epicatechin-3,5-di-O-gallate and prodelphinidin-O-gallate being among the main discriminators. The results indicate that the combined use of LC-LTQ-Orbitrap FTMS and LC-TOFMS-SPE-NMR leads to a more comprehensive metabolite description and comparison of tea and other plant samples. Sample description: Black, green, and white tea samples were obtained from different origins: a local store (bought on June 5, 2011) and a dedicated tea shop (bought on June 4, 2011) that also ordered several special tea samples at http://www.wollenhaupt.com/ (article no. in brackets) with a packaging date of May 19, 2011, indicated with an asterisk. The tea products were stored under dark conditions at room temperature until use (about 6 weeks). Tea samples were labeled as follows: green tea (GT), China Yunnan (Y) [article no. 00518]*, China Sencha (S) [article no. 00515]*, Chinese Huangshan Green Tea from laboratory (GL) (local store), China Bancha (B) [article no. 00568], China Chun Mee (CCM) [article no. 00500]*, China Lung Ching (CLC), China Gunpowder (CG); white tea (WT), China Mao Feng (CMF) [article no. 00519]*, China Pai Mu Tan (PMT) [article no. 00509]*, Jasmijn and Oranjebloesem (WTJ) (local store); black tea (BT), Darjeeling FTGFOP1 (D) [article no. 00312]*, Ceylon OP Adawatte (CAD) [article no. 00203]*, Assam TGFOP1 Hazelbank (A) [article no. 00109]*, English Earl Gray–Ceylon Black Tea with bergamot (CB) [article no. 10861], Irish Breakfast (IB) [article no. 00418], Ceylon OP Pettiagalla (CP) [article no. 00209], Pickwick English Tea Blend (BL) (local store).