#METABOLOMICS WORKBENCH epannkuk_20240711_062357 DATATRACK_ID:4998 STUDY_ID:ST003334 ANALYSIS_ID:AN005463 PROJECT_ID:PR002073
VERSION             	1
CREATED_ON             	July 17, 2024, 5:09 am
#PROJECT
PR:PROJECT_TITLE                 	Impact of partial body shielding from very high dose rates on untargeted
PR:PROJECT_TITLE                 	metabolomics in biodosimetry
PR:PROJECT_SUMMARY               	A realistic exposure to ionizing radiation (IR) from an improvised nuclear
PR:PROJECT_SUMMARY               	device will likely include individuals that are partially shielded from the
PR:PROJECT_SUMMARY               	initial blast delivered at a very high-dose rate (VHDR). As different tissues
PR:PROJECT_SUMMARY               	have varying levels of radiosensitivity, e.g. hematopoietic vs. gastrointestinal
PR:PROJECT_SUMMARY               	tissues, the effects of shielding on radiation biomarkers needs to be addressed.
PR:PROJECT_SUMMARY               	Here, we explore how biofluid (urine and serum) metabolite signatures from male
PR:PROJECT_SUMMARY               	and female C57BL/6 mice exposed to VHDR (5 – 10 Gy/sec) total body irradiation
PR:PROJECT_SUMMARY               	(TBI, 0, 4, and 8 Gy) compare to individuals exposed to partial body irradiation
PR:PROJECT_SUMMARY               	(PBI) (lower body irradiated [LBI] or upper body irradiated [UBI] at an 8 Gy
PR:PROJECT_SUMMARY               	dose) using a data-independent acquisition untargeted metabolomics approach.
PR:PROJECT_SUMMARY               	Although sex differences were observed in the spatial groupings of urine
PR:PROJECT_SUMMARY               	signatures from TBI and PBI mice, a metabolite signature
PR:PROJECT_SUMMARY               	(N6,N6,N6-trimethyllysine, carnitine, propionylcarnitine,
PR:PROJECT_SUMMARY               	hexosamine-valine-isoleucine, taurine, and creatine) previously developed from
PR:PROJECT_SUMMARY               	variable dose rate experiments was able to identify individuals with high
PR:PROJECT_SUMMARY               	sensitivity and specificity irrespective of radiation shielding. A panel of
PR:PROJECT_SUMMARY               	serum metabolites composed from previous untargeted studies on nonhuman primates
PR:PROJECT_SUMMARY               	had excellent performance for separating irradiated cohorts; however, a
PR:PROJECT_SUMMARY               	multi-omic approach to complement the metabolome could increase dose estimation
PR:PROJECT_SUMMARY               	confidence intervals. Overall, these results support the inclusion of small
PR:PROJECT_SUMMARY               	molecule markers in biodosimetry assays without substantial interference from
PR:PROJECT_SUMMARY               	upper or lower body shielding.
PR:INSTITUTE                     	Georgetown University
PR:LAST_NAME                     	Pannkuk
PR:FIRST_NAME                    	Evan
PR:ADDRESS                       	3970 Reservoir Rd, NW New Research Build, washington dc, District of Columbia,
PR:ADDRESS                       	20057, USA
PR:EMAIL                         	elp44@georgetown.edu
PR:PHONE                         	2026875650
#STUDY
ST:STUDY_TITLE                   	Impact of partial body shielding from very high dose rates on untargeted
ST:STUDY_TITLE                   	metabolomics in biodosimetry
ST:STUDY_SUMMARY                 	A realistic exposure to ionizing radiation (IR) from an improvised nuclear
ST:STUDY_SUMMARY                 	device will likely include individuals that are partially shielded from the
ST:STUDY_SUMMARY                 	initial blast delivered at a very high-dose rate (VHDR). As different tissues
ST:STUDY_SUMMARY                 	have varying levels of radiosensitivity, e.g. hematopoietic vs. gastrointestinal
ST:STUDY_SUMMARY                 	tissues, the effects of shielding on radiation biomarkers needs to be addressed.
ST:STUDY_SUMMARY                 	Here, we explore how biofluid (urine and serum) metabolite signatures from male
ST:STUDY_SUMMARY                 	and female C57BL/6 mice exposed to VHDR (5 – 10 Gy/sec) total body irradiation
ST:STUDY_SUMMARY                 	(TBI, 0, 4, and 8 Gy) compare to individuals exposed to partial body irradiation
ST:STUDY_SUMMARY                 	(PBI) (lower body irradiated [LBI] or upper body irradiated [UBI] at an 8 Gy
ST:STUDY_SUMMARY                 	dose) using a data-independent acquisition untargeted metabolomics approach.
ST:STUDY_SUMMARY                 	Although sex differences were observed in the spatial groupings of urine
ST:STUDY_SUMMARY                 	signatures from TBI and PBI mice, a metabolite signature
ST:STUDY_SUMMARY                 	(N6,N6,N6-trimethyllysine, carnitine, propionylcarnitine,
ST:STUDY_SUMMARY                 	hexosamine-valine-isoleucine, taurine, and creatine) previously developed from
ST:STUDY_SUMMARY                 	variable dose rate experiments was able to identify individuals with high
ST:STUDY_SUMMARY                 	sensitivity and specificity irrespective of radiation shielding. A panel of
ST:STUDY_SUMMARY                 	serum metabolites composed from previous untargeted studies on nonhuman primates
ST:STUDY_SUMMARY                 	had excellent performance for separating irradiated cohorts; however, a
ST:STUDY_SUMMARY                 	multi-omic approach to complement the metabolome could increase dose estimation
ST:STUDY_SUMMARY                 	confidence intervals. Overall, these results support the inclusion of small
ST:STUDY_SUMMARY                 	molecule markers in biodosimetry assays without substantial interference from
ST:STUDY_SUMMARY                 	upper or lower body shielding.
ST:INSTITUTE                     	Georgetown University
ST:LAST_NAME                     	Pannkuk
ST:FIRST_NAME                    	Evan
ST:ADDRESS                       	3970 Reservoir Rd, NW New Research Build, washington dc, District of Columbia,
ST:ADDRESS                       	20057, USA
ST:EMAIL                         	elp44@georgetown.edu
ST:PHONE                         	2026875650
#SUBJECT
SU:SUBJECT_TYPE                  	Mammal
SU:SUBJECT_SPECIES               	Mus musculus
SU:TAXONOMY_ID                   	10090
SU:GENDER                        	Male and female
#SUBJECT_SAMPLE_FACTORS:         	SUBJECT(optional)[tab]SAMPLE[tab]FACTORS(NAME:VALUE pairs separated by |)[tab]Raw file names and additional sample data
SUBJECT_SAMPLE_FACTORS           	8Gy24	POS_009	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy27	POS_010	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL5	POS_011	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy7	POS_012	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	CTL2	POS_013	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy12	POS_014	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy23	POS_015	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy17	POS_016	Sample source:Serum | Sex:M | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy6	POS_017	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy18	POS_018	Sample source:Serum | Sex:M | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL1	POS_022	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy6	POS_023	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	CTL5	POS_024	Sample source:Serum | Sex:M | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy19	POS_025	Sample source:Serum | Sex:M | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy23	POS_026	Sample source:Serum | Sex:M | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL4	POS_027	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy30	POS_028	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy15	POS_029	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy20	POS_030	Sample source:Serum | Sex:M | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL1	POS_031	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy11	POS_036	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy9	POS_037	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy8	POS_038	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	CTL1	POS_039	Sample source:Serum | Sex:M | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	CTL4	POS_040	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy6	POS_041	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy21	POS_042	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL2	POS_043	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy8	POS_044	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy22	POS_045	Sample source:Serum | Sex:M | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy7	POS_049	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy12	POS_050	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy22	POS_051	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy13	POS_052	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy11	POS_053	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy10	POS_054	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy18	POS_055	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy16	POS_056	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy14	POS_057	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy9	POS_058	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy21	POS_063	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy25	POS_064	Sample source:Serum | Sex:M | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy25	POS_065	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL4	POS_066	Sample source:Serum | Sex:M | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy15	POS_067	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy29	POS_068	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy13	POS_069	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy23	POS_070	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy26	POS_071	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy10	POS_072	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy28	POS_076	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL3	POS_077	Sample source:Serum | Sex:M | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy10	POS_078	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy12	POS_079	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL3	POS_080	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy17	POS_081	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy25	POS_082	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy22	POS_083	Sample source:Serum | Sex:F | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy9	POS_084	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	CTL2	POS_085	Sample source:Serum | Sex:M | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy24	POS_090	Sample source:Serum | Sex:M | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy14	POS_091	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy7	POS_092	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy14	POS_093	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy13	POS_094	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy16	POS_095	Sample source:Serum | Sex:M | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy21	POS_096	Sample source:Serum | Sex:M | Exposure:LB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	4Gy8	POS_097	Sample source:Serum | Sex:F | Exposure:TB | Irradiation:4Gy	
SUBJECT_SAMPLE_FACTORS           	CTL3	POS_098	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy20	POS_099	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy24	POS_103	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy19	POS_104	Sample source:Serum | Sex:F | Exposure:UB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	8Gy15	POS_105	Sample source:Serum | Sex:M | Exposure:TB | Irradiation:8Gy	
SUBJECT_SAMPLE_FACTORS           	CTL5	POS_106	Sample source:Serum | Sex:F | Exposure:No exposure | Irradiation:0Gy	
#COLLECTION
CO:COLLECTION_SUMMARY            	Serum samples were prepared using BD Microtainer Tube (REF 365967) with ~100 µL
CO:COLLECTION_SUMMARY            	of whole blood added to each tube, kept at room temperature for 30 min, then
CO:COLLECTION_SUMMARY            	spun at 1300× g at 4 °C for 10 min. Serum was stored at −80 °C and then
CO:COLLECTION_SUMMARY            	shipped on dry ice to Georgetown University Medical Center
CO:SAMPLE_TYPE                   	Blood (serum)
CO:STORAGE_CONDITIONS            	-80℃
#TREATMENT
TR:TREATMENT_SUMMARY             	All animal experiments were approved by the Columbia University Institutional
TR:TREATMENT_SUMMARY             	Animal Care and Use Committee (IACUC, protocol #AABA9603) and were conducted
TR:TREATMENT_SUMMARY             	under all relevant federal and state guidelines. Male (n=5) and female (n=10)
TR:TREATMENT_SUMMARY             	C57BL/6 mice (ages 12 – 14 weeks) were purchased from Charles River
TR:TREATMENT_SUMMARY             	Laboratories (Frederick, MD) and randomly assigned to the zero-dose sham (0 Gy)
TR:TREATMENT_SUMMARY             	and irradiated (4 and 8 Gy, total and partial body exposure) cohorts. Samples
TR:TREATMENT_SUMMARY             	were collected at 1 day.
#SAMPLEPREP
SP:SAMPLEPREP_SUMMARY            	A 5 μl aliquot of serum was mixed with 195 μl of cold 66% acetonitrile
SP:SAMPLEPREP_SUMMARY            	containing internal standards (2 μM debrisoquine [M+H]+ = 176.1188; 5 μM
SP:SAMPLEPREP_SUMMARY            	chlorpropamide [M+H]+ = 277.0414, [M-H]- = 275.0257; 30 μM 4-nitrobenzoic acid
SP:SAMPLEPREP_SUMMARY            	[M-H]- = 166.0141). The samples were vortexed and then incubated on ice for 10
SP:SAMPLEPREP_SUMMARY            	min. Residual solids were pelleted to the bottom by centrifugation for 10 min
SP:SAMPLEPREP_SUMMARY            	(10,000 x g, 4°C), and then an aliquot was placed in a liquid chromatography
SP:SAMPLEPREP_SUMMARY            	(LC) vial.
#CHROMATOGRAPHY
CH:CHROMATOGRAPHY_SUMMARY        	The LC and MS conditions for serum was as follows: LC solvent A (water/0.1%
CH:CHROMATOGRAPHY_SUMMARY        	formic acid [FA]), solvent B (acetonitrile/0.1% FA), and solvent C
CH:CHROMATOGRAPHY_SUMMARY        	(isopropanol/0.1% FA). Operating conditions for ESI were, capillary voltage 3
CH:CHROMATOGRAPHY_SUMMARY        	kV, cone voltage 30 V, desolvation temperature 500°C, desolvation gas flow 600
CH:CHROMATOGRAPHY_SUMMARY        	L/Hr. The gradient for serum was: 4 min 98% A 2% B, 4 min 40% A 60% B, 1.5 min
CH:CHROMATOGRAPHY_SUMMARY        	2% A 98% B, 2 min 11.8% B 88.2% C, 0.5 min 50% A 50% B, and 1 min 98% A 2% B at
CH:CHROMATOGRAPHY_SUMMARY        	a flow rate of 0.5 ml/min, column temp 60 °C (S3 Fig).
CH:CHROMATOGRAPHY_TYPE           	Reversed phase
CH:INSTRUMENT_NAME               	Waters Acquity
CH:COLUMN_NAME                   	Waters ACQUITY UPLC BEH C18 (50 x 2.1mm,1.7um)
CH:SOLVENT_A                     	100% water; 0.1% formic acid
CH:SOLVENT_B                     	100% acetonitrile; 0.1% formic acid
CH:SOLVENT_C                     	100% isopropanol; 0.1% formic acid
CH:FLOW_GRADIENT                 	4 min 98% A 2% B, 4 min 40% A 60% B, 1.5 min 2% A 98% B, 2 min 11.8% B 88.2% C,
CH:FLOW_GRADIENT                 	0.5 min 50% A 50% B, and 1 min 98% A 2% B
CH:FLOW_RATE                     	0.5 ml/min
CH:COLUMN_TEMPERATURE            	60
#ANALYSIS
AN:ANALYSIS_TYPE                 	MS
#MS
MS:INSTRUMENT_NAME               	Waters Xevo-G2-S
MS:INSTRUMENT_TYPE               	QTRAP
MS:MS_TYPE                       	ESI
MS:ION_MODE                      	NEGATIVE
MS:MS_COMMENTS                   	Operating conditions for ESI were, capillary voltage 3 kV, cone voltage 30 V,
MS:MS_COMMENTS                   	desolvation temperature 500°C, desolvation gas flow 600 L/Hr.
MS:MS_RESULTS_FILE               	ST003334_AN005463_Results.txt	UNITS:peak area	Has m/z:Yes	Has RT:Yes	RT units:Minutes
#END