#METABOLOMICS WORKBENCH murra668_20240801_090052 DATATRACK_ID:5071 STUDY_ID:ST003500 ANALYSIS_ID:AN005745 PROJECT_ID:PR002146
VERSION             	1
CREATED_ON             	August 13, 2024, 7:38 am
#PROJECT
PR:PROJECT_TITLE                 	A UHPLC-MS/MS Method for Profiling of Urinary Mercapturic Acids using Positive
PR:PROJECT_TITLE                 	Ion Mode
PR:PROJECT_SUMMARY               	We describe an analytical global profiling approach with machine learning
PR:PROJECT_SUMMARY               	predicted structural annotations for the characterization of mercapturic acids,
PR:PROJECT_SUMMARY               	a detoxification product of chemical environmental exposure.
PR:INSTITUTE                     	University of Minnesota
PR:DEPARTMENT                    	School of Public Health, Division of Environmental Health Sciences
PR:LABORATORY                    	Balbo Research Group
PR:LAST_NAME                     	Murray
PR:FIRST_NAME                    	Kevin
PR:ADDRESS                       	2-210 CCRB, 2231 6th St SE, Minneapolis, MN 55455
PR:EMAIL                         	murra668@umn.edu
PR:PHONE                         	612-626-2182
PR:FUNDING_SOURCE                	National Cancer Institute (5R01CA222005-05)
#STUDY
ST:STUDY_TITLE                   	A UHPLC-MS/MS Method for Profiling of Urinary Mercapturic Acids using Positive
ST:STUDY_TITLE                   	Ion Mode
ST:STUDY_SUMMARY                 	We report the first application of a UHPLC-MS/MS method using positive ion mode
ST:STUDY_SUMMARY                 	detection for the unbiased characterization of mercapturic acids. The proposed
ST:STUDY_SUMMARY                 	method utilizes a neutral loss monitoring paradigm to monitor for two diagnostic
ST:STUDY_SUMMARY                 	fragmentation pathways for this class of compound. Using a cohort of 20
ST:STUDY_SUMMARY                 	nonsmokers and 20 smokers, we detected 180 putative mercapturic acid signatures
ST:STUDY_SUMMARY                 	that exhibited a high degree of reproducibility from the complex urine
ST:STUDY_SUMMARY                 	metabolome background. Following a combination of multivariate and univariate
ST:STUDY_SUMMARY                 	statistics, we found 33 putative mercapturic acids associated with smoking
ST:STUDY_SUMMARY                 	status.
ST:INSTITUTE                     	University of Minnesota
ST:LAST_NAME                     	Murray
ST:FIRST_NAME                    	Kevin
ST:ADDRESS                       	2-210 CCRB, 2231 6th St SE, Minneapolis, MN 55455
ST:EMAIL                         	murra668@umn.edu
ST:PHONE                         	612-626-2182
ST:NUM_GROUPS                    	2
ST:TOTAL_SUBJECTS                	20
#SUBJECT
SU:SUBJECT_TYPE                  	Human
SU:SUBJECT_SPECIES               	Homo sapiens
SU:TAXONOMY_ID                   	9606
SU:AGE_OR_AGE_RANGE              	21-61
SU:GENDER                        	Male and female
SU:HUMAN_SMOKING_STATUS          	Smoking and Nonsmoking
#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           	79	N079	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=3; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N079
SUBJECT_SAMPLE_FACTORS           	82	N082	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=3; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N082
SUBJECT_SAMPLE_FACTORS           	87	N087	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=8; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N087
SUBJECT_SAMPLE_FACTORS           	88	N088	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=8; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N088
SUBJECT_SAMPLE_FACTORS           	94	N094	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=12; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N094
SUBJECT_SAMPLE_FACTORS           	96	N096	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=12; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N096
SUBJECT_SAMPLE_FACTORS           	128	N128	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=17; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N128
SUBJECT_SAMPLE_FACTORS           	133	N133	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=17; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N133
SUBJECT_SAMPLE_FACTORS           	134	N134	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=22; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N134
SUBJECT_SAMPLE_FACTORS           	140	N140	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=22; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N140
SUBJECT_SAMPLE_FACTORS           	141	N141	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=24; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N141
SUBJECT_SAMPLE_FACTORS           	142	N142	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=24; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N142
SUBJECT_SAMPLE_FACTORS           	149	N149	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=20; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N149
SUBJECT_SAMPLE_FACTORS           	161	N161	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=20; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N161
SUBJECT_SAMPLE_FACTORS           	162	N162	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=15; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N162
SUBJECT_SAMPLE_FACTORS           	167	N167	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=10; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N167
SUBJECT_SAMPLE_FACTORS           	189	N189	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=15; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N189
SUBJECT_SAMPLE_FACTORS           	194	N194	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=10; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N194
SUBJECT_SAMPLE_FACTORS           	207	N207	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_1; Injection order=5; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_N207
SUBJECT_SAMPLE_FACTORS           	215	N215	Sample source:Urine | Smoking Status:Non-Smoker	Batch=Batch_2; Injection order=5; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_N215
SUBJECT_SAMPLE_FACTORS           	pool_01	pool_01	Sample source:Urine | Smoking Status:QC	Batch=Batch_1; Injection order=1; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_pool_01
SUBJECT_SAMPLE_FACTORS           	pool_02	pool_02	Sample source:Urine | Smoking Status:QC	Batch=Batch_1; Injection order=7; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_pool_02
SUBJECT_SAMPLE_FACTORS           	pool_03	pool_03	Sample source:Urine | Smoking Status:QC	Batch=Batch_1; Injection order=13; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_pool_03
SUBJECT_SAMPLE_FACTORS           	pool_04	pool_04	Sample source:Urine | Smoking Status:QC	Batch=Batch_1; Injection order=19; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_pool_04
SUBJECT_SAMPLE_FACTORS           	pool_05	pool_05	Sample source:Urine | Smoking Status:QC	Batch=Batch_1; Injection order=25; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_pool_05
SUBJECT_SAMPLE_FACTORS           	pool_06	pool_06	Sample source:Urine | Smoking Status:QC	Batch=Batch_2; Injection order=1; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_pool_06
SUBJECT_SAMPLE_FACTORS           	pool_07	pool_07	Sample source:Urine | Smoking Status:QC	Batch=Batch_2; Injection order=7; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_pool_07
SUBJECT_SAMPLE_FACTORS           	pool_08	pool_08	Sample source:Urine | Smoking Status:QC	Batch=Batch_2; Injection order=13; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_pool_08
SUBJECT_SAMPLE_FACTORS           	pool_09	pool_09	Sample source:Urine | Smoking Status:QC	Batch=Batch_2; Injection order=19; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_pool_09
SUBJECT_SAMPLE_FACTORS           	pool_10	pool_10	Sample source:Urine | Smoking Status:QC	Batch=Batch_2; Injection order=25; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_pool_10
SUBJECT_SAMPLE_FACTORS           	102	S102	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=2; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S102
SUBJECT_SAMPLE_FACTORS           	110	S110	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=2; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S110
SUBJECT_SAMPLE_FACTORS           	117	S117	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=6; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S117
SUBJECT_SAMPLE_FACTORS           	131	S131	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=6; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S131
SUBJECT_SAMPLE_FACTORS           	132	S132	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=11; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S132
SUBJECT_SAMPLE_FACTORS           	135	S135	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=11; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S135
SUBJECT_SAMPLE_FACTORS           	136	S136	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=16; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S136
SUBJECT_SAMPLE_FACTORS           	138	S138	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=16; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S138
SUBJECT_SAMPLE_FACTORS           	144	S144	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=21; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S144
SUBJECT_SAMPLE_FACTORS           	145	S145	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=21; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S145
SUBJECT_SAMPLE_FACTORS           	146	S146	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=23; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S146
SUBJECT_SAMPLE_FACTORS           	147	S147	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=23; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S147
SUBJECT_SAMPLE_FACTORS           	150	S150	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=18; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S150
SUBJECT_SAMPLE_FACTORS           	151	S151	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=18; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S151
SUBJECT_SAMPLE_FACTORS           	152	S152	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=14; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S152
SUBJECT_SAMPLE_FACTORS           	156	S156	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=14; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S156
SUBJECT_SAMPLE_FACTORS           	157	S157	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=9; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S157
SUBJECT_SAMPLE_FACTORS           	163	S163	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=9; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S163
SUBJECT_SAMPLE_FACTORS           	171	S171	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_2; Injection order=4; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230512_S171
SUBJECT_SAMPLE_FACTORS           	190	S190	Sample source:Urine | Smoking Status:Smoker	Batch=Batch_1; Injection order=4; RAW_FILE_NAME(Raw file name)=balbo006_mckeo093_19145_20230510_S190
#COLLECTION
CO:COLLECTION_SUMMARY            	Adult participants were recruited as part of an ongoing study conducted at the
CO:COLLECTION_SUMMARY            	University of Minnesota. Demographic information including gender, race, age,
CO:COLLECTION_SUMMARY            	and tobacco usage was obtained through a questionnaire. Urine samples were
CO:COLLECTION_SUMMARY            	collected throughout a 24-hour period and stored at -80 °C until the LC-MS/MS
CO:COLLECTION_SUMMARY            	analysis. Urine samples were normalized by total 24-hour collection volume prior
CO:COLLECTION_SUMMARY            	to sample preparation. Urinary creatinine levels measured using the RayBio
CO:COLLECTION_SUMMARY            	Creatinine Assay kit (RayBiotech, Norcross, GA). This study was approved by the
CO:COLLECTION_SUMMARY            	University of Minnesota Institutional Review Board.
CO:SAMPLE_TYPE                   	Urine
CO:STORAGE_CONDITIONS            	-80℃
#TREATMENT
TR:TREATMENT_SUMMARY             	Urine samples were collected from non smokers and smokers. Urine samples were
TR:TREATMENT_SUMMARY             	collected from patients over a 24-hour period. Sample were snap frozen after
TR:TREATMENT_SUMMARY             	collection. No additional sample treatment was applied.
#SAMPLEPREP
SP:SAMPLEPREP_SUMMARY            	Urine samples (200 μL) were acidified using 40 μL of a 30% aqueous HCl
SP:SAMPLEPREP_SUMMARY            	solution and vortexed gently. A mixture of 10 ng D5-PhMA, 20 ng D3-2CaEMA, 20 ng
SP:SAMPLEPREP_SUMMARY            	D3-2CyEMA, 10 ng D3-2HPMA, 50 ng D3-3HPMA, and 50 ng D3-3HMPMA was added to each
SP:SAMPLEPREP_SUMMARY            	sample. Oasis MAX mixed mode reverse phase anion exchange solid phase extraction
SP:SAMPLEPREP_SUMMARY            	cartridges (60 mg, 60 u, 2 mL reservoir size) were obtained from Waters Corp.
SP:SAMPLEPREP_SUMMARY            	(Milford, MA, USA). Before sample introduction, the plate was preconditioned
SP:SAMPLEPREP_SUMMARY            	with MeOH, water, and 2% aqueous NH4OH solutions. The samples were applied and
SP:SAMPLEPREP_SUMMARY            	washed with 0.7 mL 2% aqueous NH4OH and 0.7 mL MeOH, then dried with nitrogen
SP:SAMPLEPREP_SUMMARY            	gas for 20 min. The plate was washed with 0.7 mL 2% aqueous formic acid before
SP:SAMPLEPREP_SUMMARY            	sample collection. Finally, the unfractionated urine extracts were collected
SP:SAMPLEPREP_SUMMARY            	using 0.7 mL 90% MeOH in 2% formic acid wash. The samples were transferred from
SP:SAMPLEPREP_SUMMARY            	the 96-well collection plate to fresh 1.2 mL silanized vials and dried to
SP:SAMPLEPREP_SUMMARY            	completeness in a SpeedVac without heat. The dried samples were stored at -80
SP:SAMPLEPREP_SUMMARY            	°C until ready for LC-MS/MS analysis.
SP:PROCESSING_STORAGE_CONDITIONS 	Room temperature
SP:EXTRACT_STORAGE               	-80℃
#CHROMATOGRAPHY
CH:CHROMATOGRAPHY_TYPE           	Reversed phase
CH:INSTRUMENT_NAME               	Thermo Dionex Ultimate 3000 RS
CH:COLUMN_NAME                   	Self-packed C18 column Dr. Maisch GmbH ReproSil-PUR (450 mm x 100 µm, 1.9 µm,
CH:COLUMN_NAME                   	120 Å C18aq)
CH:SOLVENT_A                     	99.9% water; 0.1% formic acid
CH:SOLVENT_B                     	99.9% acetonitrile; 0.1% formic acid
CH:FLOW_GRADIENT                 	Chromatographic separation was performed using a linear gradient starting at 0%
CH:FLOW_GRADIENT                 	B and increased to 50% B at 40 min, 90% B at 60 min, and held for 8 min followed
CH:FLOW_GRADIENT                 	by a return to starting conditions.
CH:FLOW_RATE                     	325 nL/min
CH:COLUMN_TEMPERATURE            	55 °C
CH:METHODS_FILENAME              	MA_18786_hcdOT_30K_CNL-MS3-50CE_77min_20230510
CH:SAMPLE_INJECTION              	1% sample equivalent load in 1 μL reconstituted using a load solvent mixture of
CH:SAMPLE_INJECTION              	0.1% aqueous formic acid.
CH:ANALYTICAL_TIME               	68 min
CH:SAMPLE_LOOP_SIZE              	10 µL injection loop
#ANALYSIS
AN:ANALYSIS_TYPE                 	MS
AN:LABORATORY_NAME               	Center for Metabolomics and Proteomics
AN:OPERATOR_NAME                 	Kevin Murray
AN:DETECTOR_TYPE                 	Orbitrap
AN:ACQUISITION_DATE              	2023-05-12
AN:DATA_FORMAT                   	.RAW
#MS
MS:INSTRUMENT_NAME               	Thermo Orbitrap Fusion Tribrid
MS:INSTRUMENT_TYPE               	Orbitrap
MS:MS_TYPE                       	ESI
MS:ION_MODE                      	POSITIVE
MS:MS_COMMENTS                   	Discovery DDA-CNL-MS3 analyses of experimental samples were performed using
MS:MS_COMMENTS                   	full-scan detection followed by data-dependent MS2 acquisition and a conditional
MS:MS_COMMENTS                   	neutral loss-triggered MS3 acquisition. All analyses were performed in positive
MS:MS_COMMENTS                   	ion mode. Full-scan detection was performed using Orbitrap detection at a
MS:MS_COMMENTS                   	resolution of 120,000, AGC targeted setting of 4 × 105, a maximum ion injection
MS:MS_COMMENTS                   	time of 50 ms, and an S-Lens RF setting of 40%. Scan ranges of 170 m/z – 600
MS:MS_COMMENTS                   	m/z were used for full-scan detection. MS2 spectra were collected using a DDA
MS:MS_COMMENTS                   	design with a 2 sec cycle time in centroid mode with a 15 sec dynamic exclusion
MS:MS_COMMENTS                   	list. Fragment spectra were acquired with quadrupole isolation of 0.8 m/z,
MS:MS_COMMENTS                   	Orbitrap detection at a resolution of 30,000, an AGC setting of 1 × 105, and a
MS:MS_COMMENTS                   	100 ms maximum injection time. The analysis utilized HCD fragmentation at a
MS:MS_COMMENTS                   	fixed collision energy of 30%. MS3 spectra were collected using a conditional
MS:MS_COMMENTS                   	neutral loss design that acquired an additional fragmentation scan on ions
MS:MS_COMMENTS                   	exhibiting a neutral loss of 131.0582 Da or 105.0426 Da from the selected
MS:MS_COMMENTS                   	precursor. MS3 spectra were acquired with a full-scan MS isolation of 1.5 m/z
MS:MS_COMMENTS                   	and MS2 isolation of 2.0 m/z, Orbitrap detection at a resolution of 30,000, AGC
MS:MS_COMMENTS                   	setting of 2 × 105, and a 200 ms maximum injection time. The MS3 analysis
MS:MS_COMMENTS                   	utilized HCD fragmentation at a fixed collision energy of 50%. Data processing:
MS:MS_COMMENTS                   	Fragmentation filtering was performed using the DFBuilder module incorporated in
MS:MS_COMMENTS                   	the open-source software MZmine to monitor diagnostic neutral loss and fragment
MS:MS_COMMENTS                   	ions characteristic of mercapturic acid conjugates. Putative mercapturic acid
MS:MS_COMMENTS                   	detection required the observation of a neutral loss of 131.0582 Da (C5H9NO3) or
MS:MS_COMMENTS                   	105.0426 Da (C3H7NO3) in acquired MS/MS spectrum. A complete list of the
MS:MS_COMMENTS                   	processing parameters is summarized in Table S2. Fragmentation filtering using
MS:MS_COMMENTS                   	the DFBuilder module was performed for the specified neutral loss using a 5 ppm
MS:MS_COMMENTS                   	mass tolerance and minimum fragment ion intensity of 1 x 104 with a 1% base peak
MS:MS_COMMENTS                   	threshold. A targeted chromatogram was drawn around detected precursor masses
MS:MS_COMMENTS                   	using a 1.0 min retention time window. Masses of interest were detected using
MS:MS_COMMENTS                   	the centroid detector and noise threshold of 1 x 105. Chromatogram traces were
MS:MS_COMMENTS                   	computed using the ADAP chromatogram builder module with a mass tolerance of 5
MS:MS_COMMENTS                   	ppm. Chromatographic peaks were detected using the Local Minimum search
MS:MS_COMMENTS                   	algorithm using a 30% chromatographic threshold, 0.1 min retention time minimum
MS:MS_COMMENTS                   	search range, a minimum peak height of 1 x 105, a minimum peak top/edge ratio of
MS:MS_COMMENTS                   	10, and minimum peak width tolerance of 0.1 min. Duplicate peaks were removed
MS:MS_COMMENTS                   	using a 0.1 min retention time tolerance. Feature lists were deisotoped using
MS:MS_COMMENTS                   	the 13C isotope filter module. All samples and pooled replicate feature lists
MS:MS_COMMENTS                   	were aligned using the Join Aligner module with a mass tolerance of 5 ppm and
MS:MS_COMMENTS                   	retention time tolerance of 0.4 min. Commonly observed in-source fragments,
MS:MS_COMMENTS                   	adducts, and multimer complexes were detected and removed from consideration.
MS:MS_COMMENTS                   	Missing peak annotations were replaced using the Gap-Filling algorithm. Acquired
MS:MS_COMMENTS                   	MS/MS spectra were matched against the NIST mass spectral library (version 2020)
MS:MS_COMMENTS                   	to remove unrelated metabolic signatures. Finally, the remaining features were
MS:MS_COMMENTS                   	exported as CSV files for downstream analysis.
MS:COLLISION_ENERGY              	NCE 30%
MS:FRAGMENTATION_METHOD          	HCD
MS:ION_SPRAY_VOLTAGE             	2.1 kV
MS:IONIZATION                    	ESI
MS:MASS_ACCURACY                 	5 ppm
MS:PRECURSOR_TYPE                	[M+H]+
MS:MS_RESULTS_FILE               	ST003500_AN005745_Results.txt	UNITS:Peak heights	Has m/z:Yes	Has RT:Yes	RT units:Minutes
#END