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.

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Study ID	ST001003
Study Title	A pilot study of urine metabolomics in a female subject towards an outpatient estimate of circadian phase (part I)
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 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 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:	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
SA063084	nhilic-12oct16-004	10	day2	CR
SA063085	nC18-18oct16-004	10	day2	CR
SA063086	pC18-14oct16-004	10	day2	CR
SA063087	philic-13oct16-004	10	day2	CR
SA063088	pC18-14oct16-016	10	day3	CR
SA063089	philic-13oct16-016	10	day3	CR
SA063090	nC18-18oct16-016	10	day3	CR
SA063091	nhilic-12oct16-016	10	day3	CR
SA063092	pC18-14oct16-001	11	day1	Baseline
SA063093	nhilic-12oct16-001	11	day1	Baseline
SA063094	philic-13oct16-001	11	day1	Baseline
SA063095	nC18-18oct16-001	11	day1	Baseline
SA063096	philic-13oct16-013	11	day2	Baseline
SA063097	nhilic-12oct16-013	11	day2	Baseline
SA063098	nC18-18oct16-013	11	day2	Baseline
SA063099	pC18-14oct16-013	11	day2	Baseline
SA063100	pC18-14oct16-003	13	day1	Baseline
SA063101	nhilic-12oct16-003	13	day1	Baseline
SA063102	nC18-18oct16-003	13	day1	Baseline
SA063103	philic-13oct16-003	13	day1	Baseline
SA063104	nhilic-12oct16-015	13	day2	Baseline
SA063105	nC18-18oct16-015	13	day2	Baseline
SA063106	philic-13oct16-015	13	day2	Baseline
SA063107	pC18-14oct16-015	13	day2	Baseline
SA063108	philic-13oct16-006	13	day2	CR
SA063109	nhilic-12oct16-006	13	day2	CR
SA063110	pC18-14oct16-006	13	day2	CR
SA063111	nC18-18oct16-006	13	day2	CR
SA063112	nC18-18oct16-018	13	day3	CR
SA063113	pC18-14oct16-018	13	day3	CR
SA063114	nhilic-12oct16-018	13	day3	CR
SA063115	philic-13oct16-018	13	day3	CR
SA063116	nC18-18oct16-005	16	day1	Baseline
SA063117	philic-13oct16-005	16	day1	Baseline
SA063118	nhilic-12oct16-005	16	day1	Baseline
SA063119	pC18-14oct16-005	16	day1	Baseline
SA063120	pC18-14oct16-017	16	day2	Baseline
SA063121	nhilic-12oct16-017	16	day2	Baseline
SA063122	philic-13oct16-017	16	day2	Baseline
SA063123	nC18-18oct16-017	16	day2	Baseline
SA063124	nC18-18oct16-008	16	day2	CR
SA063125	nhilic-12oct16-008	16	day2	CR
SA063126	pC18-14oct16-008	16	day2	CR
SA063127	philic-13oct16-008	16	day2	CR
SA063128	nhilic-12oct16-020	16	day3	CR
SA063129	philic-13oct16-020	16	day3	CR
SA063130	nC18-18oct16-020	16	day3	CR
SA063131	pC18-14oct16-020	16	day3	CR
SA063132	pC18-14oct16-019	18	day2	Baseline
SA063133	nC18-18oct16-019	18	day2	Baseline
SA063134	nhilic-12oct16-019	18	day2	Baseline
SA063135	philic-13oct16-019	18	day2	Baseline
SA063136	nC18-18oct16-007	19	day1	Baseline
SA063137	philic-13oct16-007	19	day1	Baseline
SA063138	pC18-14oct16-007	19	day1	Baseline
SA063139	nhilic-12oct16-007	19	day1	Baseline
SA063140	nC18-18oct16-010	19	day2	CR
SA063141	philic-13oct16-010	19	day2	CR
SA063142	pC18-14oct16-010	19	day2	CR
SA063143	nhilic-12oct16-010	19	day2	CR
SA063144	pC18-14oct16-022	19	day3	CR
SA063145	philic-13oct16-022	19	day3	CR
SA063146	nhilic-12oct16-022	19	day3	CR
SA063147	nC18-18oct16-022	19	day3	CR
SA063148	pC18-14oct16-021	20	day2	Baseline
SA063149	philic-13oct16-021	20	day2	Baseline
SA063150	nhilic-12oct16-021	20	day2	Baseline
SA063151	nC18-18oct16-021	20	day2	Baseline
SA063152	pC18-14oct16-009	22	day1	Baseline
SA063153	nC18-18oct16-009	22	day1	Baseline
SA063154	nhilic-12oct16-009	22	day1	Baseline
SA063155	philic-13oct16-009	22	day1	Baseline
SA063156	philic-13oct16-023	22	day2	Baseline
SA063157	nC18-18oct16-023	22	day2	Baseline
SA063158	pC18-14oct16-023	22	day2	Baseline
SA063159	nhilic-12oct16-023	22	day2	Baseline
SA063160	philic-13oct16-012	22	day2	CR
SA063161	nhilic-12oct16-012	22	day2	CR
SA063162	pC18-14oct16-012	22	day2	CR
SA063163	nC18-18oct16-012	22	day2	CR
SA063164	pC18-14oct16-014	6	day3	CR
SA063165	nhilic-12oct16-014	6	day3	CR
SA063166	philic-13oct16-014	6	day3	CR
SA063167	nC18-18oct16-014	6	day3	CR
SA063168	pC18-14oct16-002	7	day2	CR
SA063169	philic-13oct16-002	7	day2	CR
SA063170	nhilic-12oct16-002	7	day2	CR
SA063171	nC18-18oct16-002	7	day2	CR
SA063172	philic-13oct16-025	7	day4	CR
SA063173	pC18-14oct16-025	7	day4	CR
SA063174	nhilic-12oct16-025	7	day4	CR
SA063175	nC18-18oct16-025	7	day4	CR
SA063176	philic-13oct16-011	8	day2	Baseline
SA063177	nhilic-12oct16-011	8	day2	Baseline
SA063178	nC18-18oct16-011	8	day2	Baseline
SA063179	pC18-14oct16-011	8	day2	Baseline
SA063080	philic-13oct16-024	-	day4	CR
SA063081	nhilic-12oct16-024	-	day4	CR
SA063082	nC18-18oct16-024	-	day4	CR
SA063083	pC18-14oct16-024	-	day4	CR

Showing results 1 to 100 of 100

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.

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