Summary of Study ST001002

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.

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Study ID	ST001002
Study Title	A pilot study of urine metabolomics in two female and one male subject towards an outpatient estimate of circadian phase using urine storage as a factor (part II)
Study 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 elivered on ice to the processing lab, where the samples were then stored at either -20 degrees or -80 degrees (see details below). At the end of the study, samples were transported (~2 blocks) from the processing lab to our -20 or -80 freezer for storage. The samples being sent represent samples from two female subjects (3634A and 3635A) and one male subject (3624A). These subjects all spent 6 days in the lab: 3 baseline days where the subjects 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 samples from these subjects (plus 6-sulphatoxymelatonin profile) 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 Name	Hilaire
First Name	Melissa
Address	221 Longwood Avenue, Suite BL438 Boston, Massachusetts 02115
Email	msthilaire@rics.bwh.harvard.edu
Phone	617-732-4013
Submit Date	2018-07-10
Analysis Type Detail	LC-MS
Release Date	2022-12-15
Release Version	1

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:	SU001041
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
SA062580	pC18-16aug17-087	10	day1	Baseline -20 storage
SA062581	nC18-17aug17-087	10	day1	Baseline -20 storage
SA062582	nhilic-12aug17-087	10	day1	Baseline -20 storage
SA062583	philic-11aug17-087	10	day1	Baseline -20 storage
SA062584	nhilic-05aug17-014	10	day3	CR -20 storage
SA062585	pC18-04aug17-014	10	day3	CR -20 storage
SA062586	nC18-05aug17-014	10	day3	CR -20 storage
SA062587	philic-04aug17-014	10	day3	CR -20 storage
SA062588	nC18-05aug17-020	10	day4	CR -20 storage
SA062589	nhilic-05aug17-020	10	day4	CR -20 storage
SA062590	philic-04aug17-020	10	day4	CR -20 storage
SA062591	philic-14aug17-119	10	day4	CR -20 storage
SA062592	pC18-04aug17-020	10	day4	CR -20 storage
SA062593	nhilic-15aug17-119	10	day4	CR -20 storage
SA062594	nC18-19aug17-119	10	day4	CR -20 storage
SA062595	pC18-18aug17-119	10	day4	CR -20 storage
SA062596	pC18-04aug17-001	11	day1	Baseline -20 storage
SA062597	nC18-05aug17-001	11	day1	Baseline -20 storage
SA062598	nhilic-12aug17-088	11	day1	Baseline -20 storage
SA062599	nC18-17aug17-088	11	day1	Baseline -20 storage
SA062600	philic-11aug17-088	11	day1	Baseline -20 storage
SA062601	pC18-16aug17-088	11	day1	Baseline -20 storage
SA062602	philic-04aug17-001	11	day1	Baseline -20 storage
SA062603	nhilic-05aug17-001	11	day1	Baseline -20 storage
SA062604	nC18-17aug17-097	11	day2	Baseline -20 storage
SA062605	nhilic-12aug17-097	11	day2	Baseline -20 storage
SA062606	pC18-16aug17-097	11	day2	Baseline -20 storage
SA062607	nC18-11aug17-034	11	day2	Baseline -20 storage
SA062608	philic-11aug17-097	11	day2	Baseline -20 storage
SA062609	philic-07aug17-034	11	day2	Baseline -20 storage
SA062610	pC18-09aug17-034	11	day2	Baseline -20 storage
SA062611	nC18-05aug17-007	11	day2	Baseline -20 storage
SA062612	nhilic-05aug17-007	11	day2	Baseline -20 storage
SA062613	pC18-04aug17-007	11	day2	Baseline -20 storage
SA062614	nhilic-08aug17-034	11	day2	Baseline -20 storage
SA062615	philic-04aug17-007	11	day2	Baseline -20 storage
SA062616	nC18-15aug17-063	11	day2	Baseline -80 storage
SA062617	philic-09aug17-063	11	day2	Baseline -80 storage
SA062618	pC18-14aug17-063	11	day2	Baseline -80 storage
SA062619	nhilic-10aug17-063	11	day2	Baseline -80 storage
SA062620	nC18-19aug17-107	11	day3	CR -20 storage
SA062621	philic-14aug17-107	11	day3	CR -20 storage
SA062622	nhilic-15aug17-107	11	day3	CR -20 storage
SA062623	pC18-18aug17-107	11	day3	CR -20 storage
SA062624	nC18-19aug17-120	11	day4	CR -20 storage
SA062625	nhilic-15aug17-120	11	day4	CR -20 storage
SA062626	philic-14aug17-120	11	day4	CR -20 storage
SA062627	pC18-18aug17-120	11	day4	CR -20 storage
SA062628	nC18-11aug17-027	12	day1	Baseline -20 storage
SA062629	pC18-09aug17-027	12	day1	Baseline -20 storage
SA062630	philic-07aug17-027	12	day1	Baseline -20 storage
SA062631	nhilic-08aug17-027	12	day1	Baseline -20 storage
SA062632	pC18-14aug17-056	12	day1	Baseline -80 storage
SA062633	philic-09aug17-056	12	day1	Baseline -80 storage
SA062634	nC18-15aug17-056	12	day1	Baseline -80 storage
SA062635	nhilic-10aug17-056	12	day1	Baseline -80 storage
SA062636	nC18-11aug17-035	12	day2	Baseline -20 storage
SA062637	philic-07aug17-035	12	day2	Baseline -20 storage
SA062638	pC18-09aug17-035	12	day2	Baseline -20 storage
SA062639	nhilic-08aug17-035	12	day2	Baseline -20 storage
SA062640	philic-09aug17-064	12	day2	Baseline -80 storage
SA062641	nhilic-10aug17-064	12	day2	Baseline -80 storage
SA062642	pC18-14aug17-064	12	day2	Baseline -80 storage
SA062643	nC18-15aug17-064	12	day2	Baseline -80 storage
SA062644	nhilic-08aug17-044	12	day3	CR -20 storage
SA062645	pC18-09aug17-044	12	day3	CR -20 storage
SA062646	nC18-11aug17-044	12	day3	CR -20 storage
SA062647	philic-07aug17-044	12	day3	CR -20 storage
SA062648	pC18-14aug17-073	12	day3	CR -80 storage
SA062649	nhilic-10aug17-073	12	day3	CR -80 storage
SA062650	nC18-15aug17-073	12	day3	CR -80 storage
SA062651	philic-09aug17-073	12	day3	CR -80 storage
SA062652	nhilic-12aug17-089	13	day1	Baseline -20 storage
SA062653	pC18-16aug17-089	13	day1	Baseline -20 storage
SA062654	philic-11aug17-089	13	day1	Baseline -20 storage
SA062655	pC18-04aug17-002	13	day1	Baseline -20 storage
SA062656	nhilic-05aug17-002	13	day1	Baseline -20 storage
SA062657	nC18-05aug17-002	13	day1	Baseline -20 storage
SA062658	philic-04aug17-002	13	day1	Baseline -20 storage
SA062659	nC18-17aug17-089	13	day1	Baseline -20 storage
SA062660	philic-07aug17-036	13	day2	Baseline -20 storage
SA062661	nhilic-08aug17-036	13	day2	Baseline -20 storage
SA062662	nhilic-05aug17-008	13	day2	Baseline -20 storage
SA062663	pC18-04aug17-008	13	day2	Baseline -20 storage
SA062664	philic-04aug17-008	13	day2	Baseline -20 storage
SA062665	nC18-05aug17-008	13	day2	Baseline -20 storage
SA062666	nC18-11aug17-036	13	day2	Baseline -20 storage
SA062667	pC18-09aug17-036	13	day2	Baseline -20 storage
SA062668	philic-09aug17-065	13	day2	Baseline -80 storage
SA062669	pC18-14aug17-065	13	day2	Baseline -80 storage
SA062670	nC18-15aug17-065	13	day2	Baseline -80 storage
SA062671	nhilic-10aug17-065	13	day2	Baseline -80 storage
SA062672	nC18-05aug17-015	13	day3	CR -20 storage
SA062673	philic-04aug17-015	13	day3	CR -20 storage
SA062674	nhilic-05aug17-015	13	day3	CR -20 storage
SA062675	pC18-04aug17-015	13	day3	CR -20 storage
SA062676	pC18-09aug17-050	13	day4	CR -20 storage
SA062677	nhilic-08aug17-050	13	day4	CR -20 storage
SA062678	philic-07aug17-050	13	day4	CR -20 storage
SA062679	nC18-05aug17-021	13	day4	CR -20 storage

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Collection:

Collection ID:	CO001035
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:	TR001055
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.

Treatment ID:

TR001055

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:	SP001048
Sampleprep Summary:	large scale profiling

Combined analysis:

Analysis ID	AN001637	AN001638	AN001639	AN001640
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:	CH001153
Instrument Name:	Agilent 1290 Infinity
Column Name:	Waters Acquity BEH Amide (150 x 2.1mm,1.7um)
Chromatography Type:	HILIC

Chromatography ID:	CH001154
Instrument Name:	Agilent 1290 Infinity
Column Name:	Waters Acquity HSS C18 (150 x 2.1mm,1.8um)
Chromatography Type:	Reversed phase

MS:

MS ID:	MS001513
Analysis ID:	AN001637
Instrument Name:	Agilent 6550 QTOF
Instrument Type:	QTOF
MS Type:	ESI
Ion Mode:	POSITIVE

MS ID:	MS001514
Analysis ID:	AN001638
Instrument Name:	Agilent 6550 QTOF
Instrument Type:	QTOF
MS Type:	ESI
Ion Mode:	NEGATIVE

MS ID:	MS001515
Analysis ID:	AN001639
Instrument Name:	Agilent 6550 QTOF
Instrument Type:	QTOF
MS Type:	ESI
Ion Mode:	POSITIVE

MS ID:	MS001516
Analysis ID:	AN001640
Instrument Name:	Agilent 6550 QTOF
Instrument Type:	QTOF
MS Type:	ESI
Ion Mode:	NEGATIVE