Summary of Study ST002942

This data is available at the NIH Common Fund's National Metabolomics Data Repository (NMDR) website, the Metabolomics Workbench, https://www.metabolomicsworkbench.org, where it has been assigned Project ID PR001830. The data can be accessed directly via it's Project DOI: 10.21228/M85H91 This work is supported by NIH grant, U2C- DK119886.

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Study IDST002942
Study TitleTargeted analysis of short chain fatty acids for the XMaS clinical trial.
Study SummaryThe Xanthohumol microbiome and signature (XMaS) study in healthy adults was a phase I, triple-masked, placebo-controlled clinical trial in healthy adults investigating effects of a natural product supplement of gut microbiome composition and metabolism. Xanthohumol, a flavonoid from the hops plant or placebo was administered to 27 healthy adults daily for eight weeks. Fecal, plasma, and 24-hr urine collections were obtained from participants at baseline and 2-week intervals. The main objective of this study was to quantify short chain fatty acids from fecal samples of particiapnts in the XMaS trail
Institute
Oregon State University
Last NameJamieson
First NamePaige
Address307 LINUS PAULING SCIENCE CTR
Emailjamiesop@oregonstate.edu
Phone5417379804
Submit Date2023-10-22
Analysis Type DetailLC-MS
Release Date2024-01-01
Release Version1
Paige Jamieson Paige Jamieson
https://dx.doi.org/10.21228/M85H91
ftp://www.metabolomicsworkbench.org/Studies/ application/zip

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Project:

Project ID:PR001830
Project DOI:doi: 10.21228/M85H91
Project Title:Targeted analyses of microbial metabolism for the XMaS clinical trial
Project Summary:The Xanthohumol microbiome and signature (XMaS) study in healthy adults was a phase I, triple-masked, placebo-controlled clinical trial in healthy adults investigating effects of a natural product supplement of gut microbiome composition and metabolism. Xanthohumol, a flavonoid from the hops plant or placebo was administered to 27 healthy adults daily for eight weeks. Fecal, plasma, and 24-hr urine collections were obtained from participants at baseline and 2-week intervals. The main objective was to examine clinical safety and subjective tolerability of xanthohumol compared to placebo. Additional aims were to monitor biomarkers of inflammation, gut permeability, bile acid metabolism, short-chain fatty acids, and metabolism of xanthohumol.
Institute:Oregon State University
Last Name:Jamieson
First Name:Paige
Address:307 LINUS PAULING SCIENCE CTR
Email:jamiesop@oregonstate.edu
Phone:5417379804

Subject:

Subject ID:SU003055
Subject Type:Human
Subject Species:Homo sapiens
Taxonomy ID:9606

Factors:

Subject type: Human; Subject species: Homo sapiens (Factor headings shown in green)

mb_sample_id local_sample_id time_weeks intervention
SA320105s106-10 control
SA320106s112-10 control
SA320107s117-10 control
SA320108s122-10 control
SA320109s104-10 control
SA320110s126-10 control
SA320111s109-10 control
SA320112s110-10 control
SA320113s107-10 control
SA320114s114-10 control
SA320115s121-10 control
SA320116s118-10 control
SA320117s119-10 control
SA320118s101-10 treated
SA320119s111-10 treated
SA320120s131-10 treated
SA320121s102-10 treated
SA320122s123-10 treated
SA320123s124-10 treated
SA320124s116-10 treated
SA320125s130-10 treated
SA320126s127-10 treated
SA320127s115-10 treated
SA320128s103-10 treated
SA320129s113-10 treated
SA320130s129-10 treated
SA320131s105-10 treated
SA320132s121-22 control
SA320133s114-22 control
SA320134s117-22 control
SA320135s110-22 control
SA320136s119-22 control
SA320137s118-22 control
SA320138s112-22 control
SA320139s122-22 control
SA320140s109-22 control
SA320141s104-22 control
SA320142s106-22 control
SA320143s107-22 control
SA320144s126-22 control
SA320145s113-22 treated
SA320146s124-22 treated
SA320147s127-22 treated
SA320148s131-22 treated
SA320149s105-22 treated
SA320150s116-22 treated
SA320151s103-22 treated
SA320152s101-22 treated
SA320153s123-22 treated
SA320154s130-22 treated
SA320155s102-22 treated
SA320156s129-22 treated
SA320157s111-22 treated
SA320158s115-22 treated
SA320159s118-34 control
SA320160s119-34 control
SA320161s114-34 control
SA320162s112-34 control
SA320163s110-34 control
SA320164s107-34 control
SA320165s117-34 control
SA320166s122-34 control
SA320167s106-34 control
SA320168s109-34 control
SA320169s104-34 control
SA320170s121-34 control
SA320171s126-34 control
SA320172s131-34 treated
SA320173s127-34 treated
SA320174s123-34 treated
SA320175s124-34 treated
SA320176s129-34 treated
SA320177s130-34 treated
SA320178s115-34 treated
SA320179s113-34 treated
SA320180s111-34 treated
SA320181s105-34 treated
SA320182s103-34 treated
SA320183s101-34 treated
SA320184s116-34 treated
SA320185s102-34 treated
SA320186s112-46 control
SA320187s121-46 control
SA320188s122-46 control
SA320189s126-46 control
SA320190s104-46 control
SA320191s106-46 control
SA320192s107-46 control
SA320193s110-46 control
SA320194s109-46 control
SA320195s118-46 control
SA320196s117-46 control
SA320197s114-46 control
SA320198s119-46 control
SA320199s127-46 treated
SA320200s103-46 treated
SA320201s129-46 treated
SA320202s124-46 treated
SA320203s131-46 treated
SA320204s105-46 treated
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Collection:

Collection ID:CO003048
Collection Summary:Fecal samples were collected longitudinally at 2-week intervals during the 8-week study. Samples were kept on ice immediately after collection and snap-frozen, then stored in -80 freezers until processing.
Sample Type:Feces

Treatment:

Treatment ID:TR003064
Treatment Summary:Participants were randomly allocated to intervention arms to receive either 24 mg or a rice protein placebo capsule daily for 8 weeks. Clinic check-in and sample collections occurred at baseline and 2-week intervals until study close-out (week 8).

Sample Preparation:

Sampleprep ID:SP003061
Sampleprep Summary:Fecal samples were dried using vacuum desiccator and 70% methanol:water (1:4 w/v) was added for fecal homogenate. Samples were centrifuged and supernatant was collected. Supernatant was diluted 1:5 in 50% acetonitrile:water and short chain fatty acids were derivatized with 3-nitrophenylhydrazine for better resolution by LC-MS. Briefly, 40 uL of fecal supernatant was added to 20 uL 120 mM EDC, 20 uL 6% pyridine, and 20 uL 200 mM 3-NPH. The mixture was allowed to react for 30 min at 40 °C and subsequently diluted 1:200 in 10% acetonitrile:water.

Combined analysis:

Analysis ID AN004827
Analysis type MS
Chromatography type Reversed phase
Chromatography system Waters Acquity I-Class
Column Waters ACQUITY UPLC BEH C18 (100 x 2.1mm,1.7um)
MS Type ESI
MS instrument type Triple quadrupole
MS instrument name Waters Xevo TQ-XS
Ion Mode NEGATIVE
Units mg/g

Chromatography:

Chromatography ID:CH003647
Instrument Name:Waters Acquity I-Class
Column Name:Waters ACQUITY UPLC BEH C18 (100 x 2.1mm,1.7um)
Column Temperature:40
Flow Gradient:from 0 to 2 min, 15% B; from 2 to 11 min 15-55% B; from 11 to 12 min, 100% B; from 12 to 12.5 min, 100-15% B; and from 12.5 to 15 min, 15% B
Flow Rate:0.35 mL/min
Solvent A:water with 0.01% formic acid
Solvent B:acetonitrile with 0.01% formic acid
Chromatography Type:Reversed phase

MS:

MS ID:MS004573
Analysis ID:AN004827
Instrument Name:Waters Xevo TQ-XS
Instrument Type:Triple quadrupole
MS Type:ESI
MS Comments:Metabolites (acetate, propionate, butyrate, lactate, valerate) were verified by matching m/z value, retention times, and product ions of SRM transitions with those of authenticated standards. TargetLynx Application Manager was used for data processing.
Ion Mode:NEGATIVE
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