Summary of Study ST001003

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 PR000678. The data can be accessed directly via it's Project DOI: 10.21228/M81Q26 This work is supported by NIH grant, U2C- DK119886.

See: https://www.metabolomicsworkbench.org/about/howtocite.php

This study contains a large results data set and is not available in the mwTab file. It is only available for download via FTP as data file(s) here.

Show all samples  |  Perform analysis on untargeted data  
Download mwTab file (text)   |  Download mwTab file(JSON)   |  Download data files
Study IDST001003
Study TitleA pilot study of urine metabolomics in a female subject towards an outpatient estimate of circadian phase (part I)
Study SummarySerial urine samples were collected at each void (approximately every 3 hours) from subjects during a 6-day inpatient protocol. The total volume of each sample was measured, and then 5 mL was aliquoted into a 7 mL tube and delivered on ice to the processing lab, where the samples were then stored at -80 degrees. At the end of the study, samples were transported (~2 blocks) from the processing lab to our -80 freezer for storage. The samples being sent represent samples from one female subject. This subject spent 6 days in the lab: 3 baseline days where the subject slept for 8 hours at night (at habitual times as determined during the screening period) and 16 hours of ambulatory wake in ambient light, followed by 50 hours of continuous wakefulness in which the subject was kept in a semi-recumbent position in bed under dim light and fed hourly isocaloric snacks (called a constant routine). We are requesting untargeted profiling of 25 samples (sample #: 52919-52943) to determine how the concentrations of different metabolites vary across the 24-hour period, and specifically to compare this circadian variation in each metabolite during a 48-hour ambulatory period versus a 48-hour constant routine period.
Institute
Mayo Clinic
Last NameHilaire
First NameMelissa
Address221 Longwood Avenue, Suite BL438 Boston, Massachusetts 02115
Emailmsthilaire@rics.bwh.harvard.edu
Phone617-732-4013
Submit Date2018-07-10
Analysis Type DetailLC-MS
Release Date2022-12-15
Release Version1
Melissa Hilaire Melissa Hilaire
https://dx.doi.org/10.21228/M81Q26
ftp://www.metabolomicsworkbench.org/Studies/ application/zip

Select appropriate tab below to view additional metadata details:

Project:

Project ID:PR000678
Project DOI:doi: 10.21228/M81Q26
Project Title:Mayo Pilot and Feasibility: A pilot study of urine metabolomics towards an outpatient estimate of circadian phase
Project Summary:Although the effectiveness of several therapeutic interventions depend critically on their timing with respect to circadian phase, including the timing of light therapy for circadian rhythm sleep disorders, medications for high blood pressure, and chemotherapy treatments for cancer, no clinical test is available to reliably measure circadian phase rapidly, inexpensively, and non-invasively. This project will therefore provide the essential first steps toward the development and validation of a clinical test to estimate circadian phase from a single urine void via the identification of multiple rhythmic metabolites in urine using untargeted metabolomic profiling methods. Current methods to assess circadian phase in urine require serial measurement of a single compound (e.g., 6-sulphatoxymelatonin, the urinary metabolite of melatonin) over a 24- to 48-hour sampling window. Our approach proposes to assess many compounds in one sample to estimate circadian phase, based on the phase relationships across multiple parameters, an approach that is supported by our theoretical modeling framework. Using the untargeted metabolomics profiling services offered by the Mayo Clinic Metabolomics Resource Core, we will examine the 48-hour profiles of ~300 metabolites identified from urine samples collected in a randomly selected pilot sample of 12 healthy young volunteers (from >200 subjects) studied on an inpatient laboratory protocol that included both an ambulatory condition (i.e., habitual sleep-wake times under ordinary room light) and a constant routine procedure, the gold standard method for assessing circadian rhythms (i.e., 50-hour period during which subjects remain awake in a semi-recumbent posture in bed under dim light with equicaloric snacks served hourly). Cosinor analysis will be employed to determine which identified metabolites exhibit circadian rhythmicity, and comparisons between ambulatory and constantroutine conditions will further identify which metabolites are influenced by external factors such as sleep, meal timing, light, and posture. Finally, we will employ our theoretical modeling framework to estimate circadian phase from a single urine void using the concentration ratios of multiple metabolites that exhibit reliable and robust circadian rhythmicity. The accuracy of estimated circadian phase will be determined by comparison to actual circadian phase as defined by the peak of the 6-sulphatoxymelatonin rhythm. Once this approach has been established in a pilot set of subjects, future studies will focus on validation and testing of this approach in other data from our repository, including healthy young volunteers who have undergone rapid phase shift due to changes in sleep-wake schedule (i.e., simulated shift work) or in response to bright light exposure; patients with insomnia, who exhibit an 8-hour range in circadian phase; and blind participants without light perception, who exhibit non-entrained rhythms. Future studies will also test the efficacy of this method to a priori estimate circadian phase in patient populations that may benefit from improvements in circadian timing of treatment. The current proposal therefore represents the first essential step in developing a tool that can revolutionize medicine by adding an accurate measure of internal time – circadian medicine – into standard clinical practice.
Institute:Mayo Clinic
Last Name:Hilaire
First Name:Melissa
Address:221 Longwood Avenue, Suite BL438 Boston, Massachusetts 02115
Email:msthilaire@rics.bwh.harvard.edu
Phone:617-732-4013

Subject:

Subject ID:SU001042
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 Hour day Group
SA063084nhilic-12oct16-00410 day2 CR
SA063085nC18-18oct16-00410 day2 CR
SA063086pC18-14oct16-00410 day2 CR
SA063087philic-13oct16-00410 day2 CR
SA063088pC18-14oct16-01610 day3 CR
SA063089philic-13oct16-01610 day3 CR
SA063090nC18-18oct16-01610 day3 CR
SA063091nhilic-12oct16-01610 day3 CR
SA063092pC18-14oct16-00111 day1 Baseline
SA063093nhilic-12oct16-00111 day1 Baseline
SA063094philic-13oct16-00111 day1 Baseline
SA063095nC18-18oct16-00111 day1 Baseline
SA063096philic-13oct16-01311 day2 Baseline
SA063097nhilic-12oct16-01311 day2 Baseline
SA063098nC18-18oct16-01311 day2 Baseline
SA063099pC18-14oct16-01311 day2 Baseline
SA063100pC18-14oct16-00313 day1 Baseline
SA063101nhilic-12oct16-00313 day1 Baseline
SA063102nC18-18oct16-00313 day1 Baseline
SA063103philic-13oct16-00313 day1 Baseline
SA063104nhilic-12oct16-01513 day2 Baseline
SA063105nC18-18oct16-01513 day2 Baseline
SA063106philic-13oct16-01513 day2 Baseline
SA063107pC18-14oct16-01513 day2 Baseline
SA063108philic-13oct16-00613 day2 CR
SA063109nhilic-12oct16-00613 day2 CR
SA063110pC18-14oct16-00613 day2 CR
SA063111nC18-18oct16-00613 day2 CR
SA063112nC18-18oct16-01813 day3 CR
SA063113pC18-14oct16-01813 day3 CR
SA063114nhilic-12oct16-01813 day3 CR
SA063115philic-13oct16-01813 day3 CR
SA063116nC18-18oct16-00516 day1 Baseline
SA063117philic-13oct16-00516 day1 Baseline
SA063118nhilic-12oct16-00516 day1 Baseline
SA063119pC18-14oct16-00516 day1 Baseline
SA063120pC18-14oct16-01716 day2 Baseline
SA063121nhilic-12oct16-01716 day2 Baseline
SA063122philic-13oct16-01716 day2 Baseline
SA063123nC18-18oct16-01716 day2 Baseline
SA063124nC18-18oct16-00816 day2 CR
SA063125nhilic-12oct16-00816 day2 CR
SA063126pC18-14oct16-00816 day2 CR
SA063127philic-13oct16-00816 day2 CR
SA063128nhilic-12oct16-02016 day3 CR
SA063129philic-13oct16-02016 day3 CR
SA063130nC18-18oct16-02016 day3 CR
SA063131pC18-14oct16-02016 day3 CR
SA063132pC18-14oct16-01918 day2 Baseline
SA063133nC18-18oct16-01918 day2 Baseline
SA063134nhilic-12oct16-01918 day2 Baseline
SA063135philic-13oct16-01918 day2 Baseline
SA063136nC18-18oct16-00719 day1 Baseline
SA063137philic-13oct16-00719 day1 Baseline
SA063138pC18-14oct16-00719 day1 Baseline
SA063139nhilic-12oct16-00719 day1 Baseline
SA063140nC18-18oct16-01019 day2 CR
SA063141philic-13oct16-01019 day2 CR
SA063142pC18-14oct16-01019 day2 CR
SA063143nhilic-12oct16-01019 day2 CR
SA063144pC18-14oct16-02219 day3 CR
SA063145philic-13oct16-02219 day3 CR
SA063146nhilic-12oct16-02219 day3 CR
SA063147nC18-18oct16-02219 day3 CR
SA063148pC18-14oct16-02120 day2 Baseline
SA063149philic-13oct16-02120 day2 Baseline
SA063150nhilic-12oct16-02120 day2 Baseline
SA063151nC18-18oct16-02120 day2 Baseline
SA063152pC18-14oct16-00922 day1 Baseline
SA063153nC18-18oct16-00922 day1 Baseline
SA063154nhilic-12oct16-00922 day1 Baseline
SA063155philic-13oct16-00922 day1 Baseline
SA063156philic-13oct16-02322 day2 Baseline
SA063157nC18-18oct16-02322 day2 Baseline
SA063158pC18-14oct16-02322 day2 Baseline
SA063159nhilic-12oct16-02322 day2 Baseline
SA063160philic-13oct16-01222 day2 CR
SA063161nhilic-12oct16-01222 day2 CR
SA063162pC18-14oct16-01222 day2 CR
SA063163nC18-18oct16-01222 day2 CR
SA063164pC18-14oct16-0146 day3 CR
SA063165nhilic-12oct16-0146 day3 CR
SA063166philic-13oct16-0146 day3 CR
SA063167nC18-18oct16-0146 day3 CR
SA063168pC18-14oct16-0027 day2 CR
SA063169philic-13oct16-0027 day2 CR
SA063170nhilic-12oct16-0027 day2 CR
SA063171nC18-18oct16-0027 day2 CR
SA063172philic-13oct16-0257 day4 CR
SA063173pC18-14oct16-0257 day4 CR
SA063174nhilic-12oct16-0257 day4 CR
SA063175nC18-18oct16-0257 day4 CR
SA063176philic-13oct16-0118 day2 Baseline
SA063177nhilic-12oct16-0118 day2 Baseline
SA063178nC18-18oct16-0118 day2 Baseline
SA063179pC18-14oct16-0118 day2 Baseline
SA063080philic-13oct16-024- day4 CR
SA063081nhilic-12oct16-024- day4 CR
SA063082nC18-18oct16-024- day4 CR
SA063083pC18-14oct16-024- day4 CR
Showing results 1 to 100 of 100

Collection:

Collection ID:CO001036
Collection Summary:Serial urine samples were collected at each void (approximately every 3 hours) from subjects during a 6-day inpatient protocol. The total volume of each sample was measured, and then 5 mL was aliquoted into a 7 mL tube and delivered on ice to the processing lab, where the samples were then stored at -80 degrees. At the end of the study, samples were transported (~2 blocks) from the processing lab to our -80 freezer for storage.
Sample Type:Urine

Treatment:

Treatment ID:TR001056
Treatment Summary:This subject (subject code: 3635A) spent 6 days in the lab: 3 baseline days where the subject slept for 8 hours at night (at habitual times as determined during the screening period) and 16 hours of ambulatory wake in ambient light, followed by 50 hours of continuous wakefulness in which the subject was kept in a semi-recumbent position in bed under dim light and fed hourly isocaloric snacks (called a constant routine). In the study design, baseline and CR are used to group the 3 day baseline days and constant routine days.

Sample Preparation:

Sampleprep ID:SP001049
Sampleprep Summary:large scale profiling

Combined analysis:

Analysis ID AN001641 AN001642 AN001643 AN001644
Analysis type MS MS MS MS
Chromatography type HILIC HILIC Reversed phase Reversed phase
Chromatography system Agilent 1290 Infinity Agilent 1290 Infinity Agilent 1290 Infinity Agilent 1290 Infinity
Column Waters Acquity BEH Amide (150 x 2.1mm,1.7um) Waters Acquity BEH Amide (150 x 2.1mm,1.7um) Waters Acquity HSS C18 (150 x 2.1mm,1.8um) Waters Acquity HSS C18 (150 x 2.1mm,1.8um)
MS Type ESI ESI ESI ESI
MS instrument type QTOF QTOF QTOF QTOF
MS instrument name Agilent 6550 QTOF Agilent 6550 QTOF Agilent 6550 QTOF Agilent 6550 QTOF
Ion Mode POSITIVE NEGATIVE POSITIVE NEGATIVE
Units intensity intensity intensity intensity

Chromatography:

Chromatography ID:CH001155
Instrument Name:Agilent 1290 Infinity
Column Name:Waters Acquity BEH Amide (150 x 2.1mm,1.7um)
Chromatography Type:HILIC
  
Chromatography ID:CH001156
Instrument Name:Agilent 1290 Infinity
Column Name:Waters Acquity HSS C18 (150 x 2.1mm,1.8um)
Chromatography Type:Reversed phase

MS:

MS ID:MS001517
Analysis ID:AN001641
Instrument Name:Agilent 6550 QTOF
Instrument Type:QTOF
MS Type:ESI
Ion Mode:POSITIVE
  
MS ID:MS001518
Analysis ID:AN001642
Instrument Name:Agilent 6550 QTOF
Instrument Type:QTOF
MS Type:ESI
Ion Mode:NEGATIVE
  
MS ID:MS001519
Analysis ID:AN001643
Instrument Name:Agilent 6550 QTOF
Instrument Type:QTOF
MS Type:ESI
Ion Mode:POSITIVE
  
MS ID:MS001520
Analysis ID:AN001644
Instrument Name:Agilent 6550 QTOF
Instrument Type:QTOF
MS Type:ESI
Ion Mode:NEGATIVE
  logo