#METABOLOMICS WORKBENCH blfitz_20180926_213803_mwtab.txt DATATRACK_ID:1518 STUDY_ID:ST001104 ANALYSIS_ID:AN001797 PROJECT_ID:PR000716 VERSION 1 CREATED_ON December 4, 2018, 11:25 am #PROJECT PR:PROJECT_TITLE Urine Metabolite Identification PR:PROJECT_TYPE MS and MS/MS analyses PR:PROJECT_SUMMARY Structural identification of unknown metabolites in human urine PR:INSTITUTE Colorado State University PR:DEPARTMENT MIP PR:LABORATORY Belisle PR:LAST_NAME Fitzgerald PR:FIRST_NAME Bryna PR:ADDRESS 3185 Rampart Rd, Fort Collins, CO, 80521, USA PR:EMAIL blfitz@colostate.edu PR:PHONE 9704918905 PR:FUNDING_SOURCE NIH U01 AI-115619 #STUDY ST:STUDY_TITLE Seryl-leucine core 1 O-glycosylated peptide (SLC1G) identification ST:STUDY_SUMMARY An untargeted metabolomics approach was utilized to determine urinary ST:STUDY_SUMMARY metabolites that could serve as small molecule biomarkers for treatment response ST:STUDY_SUMMARY to standard tuberculosis treatment. However, the majority of metabolites that ST:STUDY_SUMMARY most accurately distinguished patient samples at time of diagnosis from those at ST:STUDY_SUMMARY one month after the start of therapy lacked structural identification. The ST:STUDY_SUMMARY detection of unknown metabolite structures is a well-known limitation of ST:STUDY_SUMMARY untargeted metabolomics, and underscores a need for continued elucidation of ST:STUDY_SUMMARY novel metabolite structures. In this study, we sought to define the structure of ST:STUDY_SUMMARY a urine metabolite with an experimentally determined mass of 202.1326 Da, ST:STUDY_SUMMARY classified as molecular feature (MF) 874.3547. Using mass spectrometry combined ST:STUDY_SUMMARY with enzymatic digestions, the metabolite was structurally characterized as a ST:STUDY_SUMMARY seryl-leucine core 1 O-glycosylated peptide (SLC1G) of human origin. ST:INSTITUTE Colorado State University ST:LAST_NAME Fitzgerald ST:FIRST_NAME Bryna ST:ADDRESS 3185 Rampart Rd ST:EMAIL blfitz@colostate.edu ST:PHONE 9704918905 #SUBJECT SU:SUBJECT_TYPE Human 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 - 7728_CE20.d Sample Type:Patient urine SUBJECT_SAMPLE_FACTORS - SL_10.d Sample Type:Seryl-leucine Standard SUBJECT_SAMPLE_FACTORS - SLC1G_only.d Sample Type:Enriched SLC1G SUBJECT_SAMPLE_FACTORS - SLC1G+a2-3.d Sample Type:Enriched SLC1G after treatment with a2-3 neuraminidase SUBJECT_SAMPLE_FACTORS - SLC1G+a2-368.d Sample Type:Enriched SLC1G after treatment with a2-3,6,8 neuraminidase SUBJECT_SAMPLE_FACTORS - SLC1G+both.d Sample Type:Enriched SLC1G after treatment with a2-3,6,8 neuraminidase and O-glycosidase SUBJECT_SAMPLE_FACTORS - SLC1G+both_10.d Sample Type:Enriched SLC1G after treatment with a2-3,6,8 neuraminidase and O-glycosidase for comparison with seryl-leucine standard SUBJECT_SAMPLE_FACTORS - SLC1G+both-r002.d Sample Type:Enriched SLC1G after treatment with a2-3,6,8 neuraminidase and O-glycosidase for comparison with seryl-leucine standard SUBJECT_SAMPLE_FACTORS - SL-r002.d Sample Type:Seryl-leucine Standard #COLLECTION CO:COLLECTION_SUMMARY Urine was collected and frozen at -20 for storage. Prior to analysis, urine was CO:COLLECTION_SUMMARY thawed and centrifuged to remove particulates. CO:SAMPLE_TYPE Urine #TREATMENT TR:TREATMENT_SUMMARY Urine, SLC1G enriched from urine, and seryl-leucine synthetic standard were TR:TREATMENT_SUMMARY analyzed by LC-MS and LC-MS/MS #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Urine was thawed on ice and centrifuged to remove particulates prior to SP:SAMPLEPREP_SUMMARY analysis. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_TYPE Reversed phase CH:INSTRUMENT_NAME Agilent 1200 CH:COLUMN_NAME Atlantis T3 reverse-phase C18 3.5µm column (2.1 by 150mm CH:FLOW_GRADIENT 100% Solvent A to 90% Solvent B CH:FLOW_RATE 0.25 ml/min CH:COLUMN_TEMPERATURE 30 CH:SOLVENT_A 0.1% Formic Acid in Water CH:SOLVENT_B 0.1% Formic Acid in Methanol #ANALYSIS AN:ANALYSIS_TYPE MS AN:ANALYSIS_PROTOCOL_FILE SLC1G_Identification_Methods AN:DATA_FORMAT .d #MS MS:MS_COMMENTS - MS:INSTRUMENT_NAME Agilent 6520 QTOF MS:INSTRUMENT_TYPE QTOF MS:MS_TYPE ESI MS:ION_MODE POSITIVE MS:CAPILLARY_VOLTAGE 2000 V MS:COLLISION_ENERGY 10 V MS:DRY_GAS_FLOW 8 L/min MS:FRAGMENT_VOLTAGE 120 V MS:NEBULIZER 45 psi MS:OCTPOLE_VOLTAGE 750 V MS:SCANNING_CYCLE 1.2 spectra/sec MS:SCANNING_RANGE 100-1700 m/z MS:SKIMMER_VOLTAGE 60 V MS:MS_RESULTS_FILE ST001104_AN001797_Results.txt UNITS:m/z Has m/z:Yes Has RT:Yes RT units:Minutes #END