#METABOLOMICS WORKBENCH kuppal2_20170217_133440_mwtab.txt DATATRACK_ID:848 STUDY_ID:ST000596 ANALYSIS_ID:AN000914 PROJECT_ID:PR000435
VERSION             	1
CREATED_ON             	April 19, 2017, 2:07 pm
#PROJECT
PR:PROJECT_TITLE                 	Characterization of CHEAR reference material PlasmaRef_20160726
PR:PROJECT_TYPE                  	Untargeted HRMS profiling
PR:PROJECT_SUMMARY               	Results from untargeted LC-HRMS analyses of pooled CHEAR reference materials.
PR:PROJECT_SUMMARY               	PlasmaRef_20160726 was analyzed with additional NIST reference materials: SRM
PR:PROJECT_SUMMARY               	1950, SRM 1957 and SRM 1958.
PR:INSTITUTE                     	Emory University School of Medicine
PR:DEPARTMENT                    	Division of Pulmonary, Allergy and Critical Care Medicine
PR:LABORATORY                    	Clinical Biomarkers Laboratory
PR:LAST_NAME                     	Walker
PR:FIRST_NAME                    	Douglas
PR:ADDRESS                       	625 Michael St. Ste 225, Atlanta, GA, 30322, USA
PR:EMAIL                         	douglas.walker@emory.edu
PR:PHONE                         	4047275984
PR:FUNDING_SOURCE                	NIEHS ES026560
#STUDY
ST:STUDY_TITLE                   	Emory University high-resolution metabolomic profiling CHEAR pooled reference
ST:STUDY_TITLE                   	materials
ST:STUDY_TYPE                    	Untargeted HRMS for cross-laboratory characterization of common reference
ST:STUDY_TYPE                    	material.
ST:STUDY_SUMMARY                 	Proper QA/QC is an essential component of any analytical procedure. The
ST:STUDY_SUMMARY                 	variability in platforms and approaches used by the untargeted cores requires
ST:STUDY_SUMMARY                 	that each lab develop specific QA/QC protocols, making cross-laboratory
ST:STUDY_SUMMARY                 	assessments challenging. To address the difference in measures across the
ST:STUDY_SUMMARY                 	untargeted cores, the untargeted quality assurance working group (UQAWG) has
ST:STUDY_SUMMARY                 	identified the importance of using the same biological reference sample across
ST:STUDY_SUMMARY                 	the different laboratories. To reach this goal, Dr. Jones and Mr. Walker of
ST:STUDY_SUMMARY                 	Emory University volunteered to take the lead in identifying vendors, requesting
ST:STUDY_SUMMARY                 	quotes, purchasing the pooled material, delivering the specified volumes to each
ST:STUDY_SUMMARY                 	of the lab hubs and storing additional material on-site at Emory University.
ST:STUDY_SUMMARY                 	Based upon discussion with the UQAWG, it was decided that each participating
ST:STUDY_SUMMARY                 	laboratory (five total) will receive 500 mL of plasma and 2000 mL of urine,
ST:STUDY_SUMMARY                 	providing sufficient volume for daily analysis over the next five years.
ST:STUDY_SUMMARY                 	Initially, NIST standard reference materials were considered; however, limited
ST:STUDY_SUMMARY                 	supply and cost makes the use of NIST materials impractical. Vendors, including
ST:STUDY_SUMMARY                 	BioreclamationIVT, Lee Biosolutions Inc and Gemini Bio-Products were contacted
ST:STUDY_SUMMARY                 	to request quotes for preparing pooled plasma and urine meeting the following
ST:STUDY_SUMMARY                 	requirements: K2EDTA recovered whole blood (plasma), equal distribution
ST:STUDY_SUMMARY                 	male/female, equal distribution of Black/Hispanic/Caucasian donors and be
ST:STUDY_SUMMARY                 	collected from greater than 40 donors. In addition, we requested all blood
ST:STUDY_SUMMARY                 	samples be collected in FDA inspected facilities, provide collection details,
ST:STUDY_SUMMARY                 	provide general demographics for each donor and be delivered in 500 mL aliquots.
ST:STUDY_SUMMARY                 	BioreclamationIVT, who also provided the biological samples for the NIH
ST:STUDY_SUMMARY                 	metabolomics ring trial, was selected as the most appropriate vendor due to the
ST:STUDY_SUMMARY                 	ability to provide the requested materials, lead-time to deliver and price. To
ST:STUDY_SUMMARY                 	date, both pools have been purchased. The urine pool was received on July 21,
ST:STUDY_SUMMARY                 	2016 and the plasma pool will be received July 26, 2016. Upon receipt, both
ST:STUDY_SUMMARY                 	pools will be stored at -80°C. Summary demographics were provided by
ST:STUDY_SUMMARY                 	BioreclamationIVT, the urine pool was created by combining urine samples from 60
ST:STUDY_SUMMARY                 	males and 60 females with an average age of 38 (range 18-60) and equal
ST:STUDY_SUMMARY                 	distribution of races. The plasma pool was created by combining recovered plasma
ST:STUDY_SUMMARY                 	obtained from 50 males and 50 females with an average age of 38.4 (range 19-72)
ST:STUDY_SUMMARY                 	and equal distribution of races. Both urine and plasma pools will be delivered
ST:STUDY_SUMMARY                 	to the lab hubs frozen in units of 500 mL. Upon receipt, plasma and urine pools
ST:STUDY_SUMMARY                 	should be aliquoted into volumes that provide sufficient material so that
ST:STUDY_SUMMARY                 	freeze-thaw of the pooled material is minimized. For unambiguous identification,
ST:STUDY_SUMMARY                 	the urine pool has been named UrineRef_20160721 and the plasma pool has been
ST:STUDY_SUMMARY                 	named PlasmaRef_20160726. The purpose of providing each untargeted lab hub with
ST:STUDY_SUMMARY                 	the pooled material is two-fold. Through analysis of UrineRef_20160721 (if study
ST:STUDY_SUMMARY                 	samples are urine) or PlasmaRef_20160726 (if study samples are plasma) in each
ST:STUDY_SUMMARY                 	batch of samples analyzed for CHEAR, it will be possible to have a common
ST:STUDY_SUMMARY                 	reference across the different lab hubs. Thus, the ability to compare analyses
ST:STUDY_SUMMARY                 	on different platforms will be greatly improved. The use of a consistent
ST:STUDY_SUMMARY                 	reference material in each batch will also facilitate reference standardization,
ST:STUDY_SUMMARY                 	a concept developed for retrospective quantification of high-resolution
ST:STUDY_SUMMARY                 	metabolomics (Go, Walker et al. 2015). Using reference standardization,
ST:STUDY_SUMMARY                 	quantification post-data acquisition is possible by referencing the pooled
ST:STUDY_SUMMARY                 	material analyzed with each series of samples. The pooled material can be
ST:STUDY_SUMMARY                 	characterized and analytes quantified using traditional analytical chemistry
ST:STUDY_SUMMARY                 	techniques, such as quantification by methods of addition or standardization
ST:STUDY_SUMMARY                 	with a certified reference material, such as NIST SRM 1950. Known concentrations
ST:STUDY_SUMMARY                 	within the pooled material can be used to determine an analyte response factor
ST:STUDY_SUMMARY                 	and calculate sample concentrations based on single-point calibration. The
ST:STUDY_SUMMARY                 	benefit of this approach is that targeted quantification is only required in the
ST:STUDY_SUMMARY                 	pooled sample (i.e. UrineRef_20160721 or PlasmaRef_20160726), chemicals selected
ST:STUDY_SUMMARY                 	for quantification do not need to be selected a priori, and population wide
ST:STUDY_SUMMARY                 	estimates of plasma chemical concentrations can be determined without having to
ST:STUDY_SUMMARY                 	re-analyze samples using a targeted approach. Current Clinical Biomarker
ST:STUDY_SUMMARY                 	Laboratory protocol requires three analytical replicates of pooled reference
ST:STUDY_SUMMARY                 	material per day (three technical replicates per analytical replicate per column
ST:STUDY_SUMMARY                 	configuration, or 18 injections/instrument-day), resulting in analyses of the
ST:STUDY_SUMMARY                 	reference material every 10 samples. Results from untargeted LC-HRMS analyses of
ST:STUDY_SUMMARY                 	pooled CHEAR reference materials. PlasmaRef_20160726 was analyzed with
ST:STUDY_SUMMARY                 	additional NIST reference materials: SRM 1950, SRM 1957 and SRM 1958.
ST:STUDY_SUMMARY                 	UrineRef_20160721 was analyzed with NIST reference materials SRM 3672 and 3673.
ST:INSTITUTE                     	Emory University School of Medicine
ST:DEPARTMENT                    	Division of Pulmonary, Allergy and Critical Care Medicine
ST:LABORATORY                    	Clincal Biomarkers Laboratory
ST:LAST_NAME                     	Walker
ST:FIRST_NAME                    	Douglas
ST:ADDRESS                       	615 Michael St. Ste 225, Atlanta, GA, 30322, USA
ST:EMAIL                         	douglas.walker@emory.edu
ST:PHONE                         	4047275984
ST:NUM_GROUPS                    	2
ST:STUDY_COMMENTS                	Only pooled material was analyzed.
#SUBJECT
SU:SUBJECT_TYPE                  	Human plasma
SU:SUBJECT_SPECIES               	Homo sapiens
SU:TAXONOMY_ID                   	9606
#SUBJECT_SAMPLE_FACTORS:         	SUBJECT(optional)[tab]SAMPLE[tab]FACTORS(NAME:VALUE pairs separated by |)[tab]Additional sample data
SUBJECT_SAMPLE_FACTORS           	-	Pla-q3June2014_1a	Type:Plasma	Description=In-house QC pool; Sample_type=Quality control
SUBJECT_SAMPLE_FACTORS           	-	Pla-q3June2014_1b	Type:Plasma	Description=In-house QC pool; Sample_type=Quality control
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_01	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_01	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_01	Type:Plasma	Description=PlasmaRef_20160726; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_01	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_02	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_02	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_02	Type:Plasma	Description=PlasmaRef_20160727; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_02	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_03	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_03	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_03	Type:Plasma	Description=PlasmaRef_20160728; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_03	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_04	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_04	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_04	Type:Plasma	Description=PlasmaRef_20160729; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_04	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_05	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_05	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_05	Type:Plasma	Description=PlasmaRef_20160730; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_05	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	Pla-q3June2014_1c	Type:Plasma	Description=In-house QC pool; Sample_type=Quality control
SUBJECT_SAMPLE_FACTORS           	-	Pla-q3June2014_1d	Type:Plasma	Description=In-house QC pool; Sample_type=Quality control
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_06	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_06	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_06	Type:Plasma	Description=PlasmaRef_20160731; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_06	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_07	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_07	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_07	Type:Plasma	Description=PlasmaRef_20160732; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_07	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_08	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_08	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_08	Type:Plasma	Description=PlasmaRef_20160733; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_08	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_09	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_09	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_09	Type:Plasma	Description=PlasmaRef_20160734; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_09	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1957_10	Type:Serum	Description=NIST SRM 1957:  Organic Contaminants in Non-Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	NIST_1958_10	Type:Serum	Description=NIST SRM 1958:  Organic Contaminants in Fortified Human Serum (Freeze-Dried); Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	ChearPlasma_10	Type:Plasma	Description=PlasmaRef_20160735; Sample_type=CHEAR Sample
SUBJECT_SAMPLE_FACTORS           	-	NIST_1950_10	Type:Plasma	Description=NIST SRM 1950: Metabolites in Frozen Human Plasma; Sample_type=NIST Reference Material
SUBJECT_SAMPLE_FACTORS           	-	Pla-q3June2014_1e	Type:Plasma	Description=In-house QC pool; Sample_type=Quality control
SUBJECT_SAMPLE_FACTORS           	-	Pla-q3June2014_1f	Type:Plasma	Description=In-house QC pool; Sample_type=Quality control
#COLLECTION
CO:COLLECTION_SUMMARY            	The plasma pool was received by Emory University on July 26, 2016 and stored at
CO:COLLECTION_SUMMARY            	-80°C. Summary demographics were provided by BioreclamationIVT. The plasma pool
CO:COLLECTION_SUMMARY            	was created by combining recovered EDTA plasma obtained from 50 males and 50
CO:COLLECTION_SUMMARY            	females with an average age of 38.4 (range 19-72) and equal distribution of
CO:COLLECTION_SUMMARY            	races. Prior to analysis, the plasma pool was aliquoted into 0.5 mL volumes t
CO:COLLECTION_SUMMARY            	For unambiguous identification, the plasma pool has been named
CO:COLLECTION_SUMMARY            	PlasmaRef_20160726.
CO:SAMPLE_TYPE                   	Human plasma
CO:ADDITIVES                     	EDTA
CO:BLOOD_SERUM_OR_PLASMA         	Plasma
#TREATMENT
TR:TREATMENT_SUMMARY             	Samples were delivered in individual units of 500 mL. Aliquots of 0.5 mL were
TR:TREATMENT_SUMMARY             	prepared after receiving the material from BioreclamationIVT and stored at -80C
#SAMPLEPREP
SP:SAMPLEPREP_SUMMARY            	Samples were prepared for metabolomics analysis using established methods
SP:SAMPLEPREP_SUMMARY            	(Johnson et al. (2010). Analyst; Go et al. (2015). Tox Sci). Prior to analysis,
SP:SAMPLEPREP_SUMMARY            	plasma aliquots were removed from storage at -80°C and thawed on ice. Each
SP:SAMPLEPREP_SUMMARY            	cryotube was then vortexed briefly to ensure homogeneity, and 50 μL was
SP:SAMPLEPREP_SUMMARY            	transferred to a clean microfuge tube. Immediately after, the plasma was treated
SP:SAMPLEPREP_SUMMARY            	with 100 μL of ice-cold LC-MS grade acetonitrile (Sigma Aldrich) containing 2.5
SP:SAMPLEPREP_SUMMARY            	μL of internal standard solution with eight stable isotopic chemicals selected
SP:SAMPLEPREP_SUMMARY            	to cover a range of chemical properties. Following addition of acetonitrile,
SP:SAMPLEPREP_SUMMARY            	plasma was equilibrated for 30 min on ice, upon which precipitated proteins were
SP:SAMPLEPREP_SUMMARY            	removed by centrifuge (16.1 ×g at 4°C for 10 min). The resulting supernatant
SP:SAMPLEPREP_SUMMARY            	(100 μL) was removed, added to a low volume autosampler vial and maintained at
SP:SAMPLEPREP_SUMMARY            	4°C until analysis (<22 h).
SP:SAMPLEPREP_PROTOCOL_ID        	HRM_SP_082016_01
SP:SAMPLEPREP_PROTOCOL_FILENAME  	EmoryUniversity_HRM_SP_082016_01.pdf
SP:SAMPLEPREP_PROTOCOL_COMMENTS  	Date effective: 30 July 2016
SP:EXTRACTION_METHOD             	2:1 acetonitrile: sample followed by vortexing and centrifugation
SP:SAMPLE_SPIKING                	2.5 uL [13C6]-D-glucose, [15N,13C5]-L-methionine, [13C5]-L-glutamic acid,
SP:SAMPLE_SPIKING                	[15N]-L-tyrosine, [3,3-13C2]-cystine, [trimethyl-13C3]-caffeine, [U-13C5,
SP:SAMPLE_SPIKING                	U-15N2]-L-glutamine, [15N]-indole
#CHROMATOGRAPHY
CH:CHROMATOGRAPHY_SUMMARY        	The C18 column is operated parallel to the HILIC column for simultaneous
CH:CHROMATOGRAPHY_SUMMARY        	analytical separation and column flushing through the use of a dual head HPLC
CH:CHROMATOGRAPHY_SUMMARY        	pump equipped with 10-port and 6-port switching valves. During operation of the
CH:CHROMATOGRAPHY_SUMMARY        	C18 method, the MS is operated in negative ion mode and 10 μL of sample is
CH:CHROMATOGRAPHY_SUMMARY        	injected onto the C18 column while the HILIC column is flushing with wash
CH:CHROMATOGRAPHY_SUMMARY        	solution. Flow rate is maintained at 0.4 mL/min until 1.5 min, increased to 0.5
CH:CHROMATOGRAPHY_SUMMARY        	mL/min at 2 min and held for 3 min. Solvent A is 100% LC-MS grade water, solvent
CH:CHROMATOGRAPHY_SUMMARY        	B is 100% LC-MS grade acetonitrile and solvent C is 10mM ammonium acetate in
CH:CHROMATOGRAPHY_SUMMARY        	LC-MS grade water. Initial mobile phase conditions are 60% A, 35% B, 5% C hold
CH:CHROMATOGRAPHY_SUMMARY        	for 0.5 min, with linear gradient to 0% A, 95% B, 5% C at 1.5 min, hold for 3.5
CH:CHROMATOGRAPHY_SUMMARY        	min, resulting in a total analytical run time of 5 min. During the flushing
CH:CHROMATOGRAPHY_SUMMARY        	phase (HILIC analytical separation), the C18 column is equilibrated with a wash
CH:CHROMATOGRAPHY_SUMMARY        	solution of 0% A, 95% B, 5% C until 2.5 min, followed by an equilibration
CH:CHROMATOGRAPHY_SUMMARY        	solution of 60% A, 35% B, 5% C for 2.5 min.
CH:CHROMATOGRAPHY_TYPE           	Reversed phase
MS:INSTRUMENT_NAME               	Thermo Fusion Orbitrap
CH:COLUMN_NAME                   	Thermo Higgins C18 (50 x 2.1mm, 3um)
CH:COLUMN_NAME                   	with Thermo Accucore C18 guard column
CH:FLOW_GRADIENT                 	A= water, B= acetontrile, C= 10mM ammonium acetate in water; 60% A, 35% B, 5% C
CH:FLOW_GRADIENT                 	hold for 0.5 min, linear gradient to 0% A, 95% B, 5% C at 1.5 min, hold for 3
CH:FLOW_GRADIENT                 	min
CH:FLOW_RATE                     	0.4 mL/min for 1.5 min; linear increase to 0.5 mL/min at 2 min held for 3 min
CH:COLUMN_TEMPERATURE            	40C
CH:METHODS_FILENAME              	20160728_c18neg_HILICposwash_FullScan_5min
CH:SOLVENT_A                     	LC-MS grade water
CH:SOLVENT_B                     	LC-MS grade acetonitrile
CH:METHODS_ID                    	10mM ammonium acetate in LC-MS grade water
CH:SAMPLE_INJECTION              	10 uL
CH:ANALYTICAL_TIME               	5 min
CH:SAMPLE_LOOP_SIZE              	15 uL
CH:SAMPLE_SYRINGE_SIZE           	25 uL
CH:CHROMATOGRAPHY_COMMENTS       	Triplicate injections for each chromatography mode
#ANALYSIS
AN:ANALYSIS_TYPE                 	MS
AN:LABORATORY_NAME               	Clinical Biomarkers Laboratory
AN:OPERATOR_NAME                 	Vilinh Tran
AN:DETECTOR_TYPE                 	Obitrap
AN:SOFTWARE_VERSION              	Xcalibur 3.0 Rev. 3
AN:ACQUISITION_DATE              	January 2015
AN:ANALYSIS_PROTOCOL_FILE        	EmoryUniversity_HRM_FusionMS_082016_01.pdf
AN:DATA_FORMAT                   	Profile
#MS
MS:INSTRUMENT_NAME               	Thermo Fusion Orbitrap
MS:INSTRUMENT_TYPE               	Orbitrap
MS:MS_TYPE                       	ESI
MS:ION_MODE                      	NEGATIVE
MS:CAPILLARY_TEMPERATURE         	300C
MS:COLLISION_GAS                 	N2
MS:DRY_GAS_FLOW                  	45
MS:DRY_GAS_TEMP                  	250C
MS:MASS_ACCURACY                 	< 3ppm
MS:SPRAY_VOLTAGE                 	-4000
MS:ACTIVATION_PARAMETER          	5e5
MS:ACTIVATION_TIME               	118ms
MS:INTERFACE_VOLTAGE             	S-Lens RF level= 69
MS:RESOLUTION_SETTING            	60,000
MS:SCANNING_RANGE                	85-1275
MS:MS_RESULTS_FILE               	ST000596_AN000914_Results.txt
#END