#METABOLOMICS WORKBENCH dmukha_20240309_152107 DATATRACK_ID:4696 STUDY_ID:ST003151 ANALYSIS_ID:AN005170 PROJECT_ID:PR001941 VERSION 1 CREATED_ON March 27, 2024, 10:47 am #PROJECT PR:PROJECT_TITLE The shutdown of NADH oxidation via Respiratory Complex I mimics fatty acid PR:PROJECT_TITLE biosynthesis inhibition PR:PROJECT_TYPE LC-MS Quantitative Analysis PR:PROJECT_SUMMARY Proliferating cancer cells actively utilize anabolic processes for biomass PR:PROJECT_SUMMARY production, including de novo biosynthesis of amino acids, nucleotides, and PR:PROJECT_SUMMARY fatty acids. The key enzyme of the fatty acid biosynthesis pathway, fatty acid PR:PROJECT_SUMMARY synthase (FASN), is widely recognized as a promising therapeutic target in PR:PROJECT_SUMMARY cancer and other health conditions. Here, we establish a metabolic signature of PR:PROJECT_SUMMARY FASN inhibition using a panel of pharmacological inhibitors (GSK2194069, PR:PROJECT_SUMMARY TVB-2640, TVB-3166, C75, cerulenin, and Fasnall). We find that the activity of PR:PROJECT_SUMMARY some commonly used FASN inhibitors is inconsistent with the metabolic signature PR:PROJECT_SUMMARY of FASN inhibition (accumulation of malonate, succinate, malonyl coenzyme A, PR:PROJECT_SUMMARY succinyl coenzyme A, and other metabolic perturbations). Moreover, we show that PR:PROJECT_SUMMARY one of these putative FASN inhibitors, Fasnall, is a respiratory Complex I PR:PROJECT_SUMMARY inhibitor that mimics FASN inhibition through NADH accumulation and consequent PR:PROJECT_SUMMARY depletion of the tricarboxylic acid cycle metabolites. We demonstrate that PR:PROJECT_SUMMARY Fasnall impairs tumor growth in several oxidative phosphorylation-dependent PR:PROJECT_SUMMARY cancer models, including combination therapy-resistant melanoma patient-derived PR:PROJECT_SUMMARY xenografts. Fasnall administration does not reproduce neurological side effects PR:PROJECT_SUMMARY in mice reported for other Complex I inhibitors. Our results have significant PR:PROJECT_SUMMARY implications for understanding the FASN role in human health and disease and PR:PROJECT_SUMMARY provide evidence of therapeutic potential for Complex I inhibitors with fast PR:PROJECT_SUMMARY systemic clearance. Our findings also highlight the continuing need for PR:PROJECT_SUMMARY validation of small molecule inhibitors to distinguish high-quality chemical PR:PROJECT_SUMMARY probes and to expand the understanding of their application. PR:INSTITUTE Wistar Institute PR:DEPARTMENT Molecular and Cellular Oncogenesis Program, Ellen and Ronald Caplan Cancer PR:DEPARTMENT Center PR:LABORATORY Schug's Lab PR:LAST_NAME Mukha PR:FIRST_NAME Dzmitry PR:ADDRESS 3601 Spruce St., Philadelphia, Pennsylvania 19104, USA PR:EMAIL dmukha@wistar.org PR:PHONE +12154956903 PR:FUNDING_SOURCE This work was supported by grants from the National Institutes of Health (NIH) PR:FUNDING_SOURCE National Cancer Institute (NCI) DP2 CA249950-01 (Z.T.S.), NIH NCI P01 CA114046 PR:FUNDING_SOURCE (Z.T.S.), Melanoma Research Foundation 717173 (Z.T.S.), and Susan G. Komen PR:FUNDING_SOURCE CCR19608782 (Z.T.S.). PR:PUBLICATIONS Submission Pending PR:CONTRIBUTORS Dzmitry Mukha, Jena Dessain, Seamus O’Connor, Katherine Pniewski, Fabrizio PR:CONTRIBUTORS Bertolazzi, Jeet Patel, Mary Mullins, Zachary T. Schug #STUDY ST:STUDY_TITLE BT474 breast cancer cell line grown in 20% D2O-containing RPMI-1640 medium ST:STUDY_TITLE treated with Fasnall and GSK2194069 ST:STUDY_TYPE Free fatty acid analysis, D2O tracing ST:STUDY_SUMMARY BT474 breast cancer cell line grown in 20% D2O-containing medium treated with ST:STUDY_SUMMARY Fasnall and GSK2194069. Cells were grown for 24 h in RPMI-1640 with 10% dialyzed ST:STUDY_SUMMARY FBS. ST:INSTITUTE Wistar Institute ST:DEPARTMENT Molecular and Cellular Oncogenesis Program, Ellen and Ronald Caplan Cancer ST:DEPARTMENT Center ST:LABORATORY Schug's Lab ST:LAST_NAME Mukha ST:FIRST_NAME Dzmitry ST:ADDRESS 3601 Spruce St, Philadelphia, PA 19104, USA ST:EMAIL dmukha@wistar.org ST:PHONE 2154956903 ST:NUM_GROUPS 7 ST:TOTAL_SUBJECTS 21 ST:PUBLICATIONS Submission Pending #SUBJECT SU:SUBJECT_TYPE Cultured cells SU:SUBJECT_SPECIES Homo sapiens SU:TAXONOMY_ID 9606 SU:AGE_OR_AGE_RANGE 60 SU:GENDER Female SU:CELL_STRAIN_DETAILS BT-474, breast cancer cell line #FACTORS #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 - 01_FFA_Blank Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA RAW_FILE_NAME(Raw File Name)=01_FFA_Blank.raw; RAW_FILE_NAME(Raw File Name)=NEG_01_FFA_Blank.mzXML; RAW_FILE_NAME(Raw File Name )=POS_01_FFA_Blank.mzXML SUBJECT_SAMPLE_FACTORS - 02_FFA_Blank Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA RAW_FILE_NAME(Raw File Name)=02_FFA_Blank.raw; RAW_FILE_NAME(Raw File Name)=NEG_02_FFA_Blank.mzXML; RAW_FILE_NAME(Raw File Name )=POS_02_FFA_Blank.mzXML SUBJECT_SAMPLE_FACTORS - 03_FFA_Blank Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA RAW_FILE_NAME(Raw File Name)=03_FFA_Blank.raw; RAW_FILE_NAME(Raw File Name)=NEG_03_FFA_Blank.mzXML; RAW_FILE_NAME(Raw File Name )=POS_03_FFA_Blank.mzXML SUBJECT_SAMPLE_FACTORS - 04_FFA_D2O_BT474_Control Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:Vehicle RAW_FILE_NAME(Raw File Name)=04_FFA_D2O_BT474_Control.raw; RAW_FILE_NAME(Raw File Name)=NEG_04_FFA_D2O_BT474_Control.mzXML; RAW_FILE_NAME(Raw File Name )=POS_04_FFA_D2O_BT474_Control.mzXML SUBJECT_SAMPLE_FACTORS - 05_FFA_D2O_BT474_GSK0001 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 nM GSK2194069 RAW_FILE_NAME(Raw File Name)=05_FFA_D2O_BT474_GSK0001.raw; RAW_FILE_NAME(Raw File Name)=NEG_05_FFA_D2O_BT474_GSK0001.mzXML; RAW_FILE_NAME(Raw File Name )=POS_05_FFA_D2O_BT474_GSK0001.mzXML SUBJECT_SAMPLE_FACTORS - 06_FFA_D2O_BT474_GSK0040 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 nM GSK2194069 RAW_FILE_NAME(Raw File Name)=06_FFA_D2O_BT474_GSK0040.raw; RAW_FILE_NAME(Raw File Name)=NEG_06_FFA_D2O_BT474_GSK0040.mzXML; RAW_FILE_NAME(Raw File Name )=POS_06_FFA_D2O_BT474_GSK0040.mzXML SUBJECT_SAMPLE_FACTORS - 07_FFA_D2O_BT474_GSK1000 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM GSK2194069 RAW_FILE_NAME(Raw File Name)=07_FFA_D2O_BT474_GSK1000.raw; RAW_FILE_NAME(Raw File Name)=NEG_07_FFA_D2O_BT474_GSK1000.mzXML; RAW_FILE_NAME(Raw File Name )=POS_07_FFA_D2O_BT474_GSK1000.mzXML SUBJECT_SAMPLE_FACTORS - 08_FFA_D2O_BT474_Fasnall01 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM Fasnall RAW_FILE_NAME(Raw File Name)=08_FFA_D2O_BT474_Fasnall01.raw; RAW_FILE_NAME(Raw File Name)=NEG_08_FFA_D2O_BT474_Fasnall01.mzXML; RAW_FILE_NAME(Raw File Name )=POS_08_FFA_D2O_BT474_Fasnall01.mzXML SUBJECT_SAMPLE_FACTORS - 09_FFA_D2O_BT474_Fasnall05 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:5 uM Fasnall RAW_FILE_NAME(Raw File Name)=09_FFA_D2O_BT474_Fasnall05.raw; RAW_FILE_NAME(Raw File Name)=NEG_09_FFA_D2O_BT474_Fasnall05.mzXML; RAW_FILE_NAME(Raw File Name )=POS_09_FFA_D2O_BT474_Fasnall05.mzXML SUBJECT_SAMPLE_FACTORS - 10_FFA_D2O_BT474_Fasnall40 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 uM Fasnall RAW_FILE_NAME(Raw File Name)=10_FFA_D2O_BT474_Fasnall40.raw; RAW_FILE_NAME(Raw File Name)=NEG_10_FFA_D2O_BT474_Fasnall40.mzXML; RAW_FILE_NAME(Raw File Name )=POS_10_FFA_D2O_BT474_Fasnall40.mzXML SUBJECT_SAMPLE_FACTORS - 11_FFA_D2O_BT474_Control Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:Vehicle RAW_FILE_NAME(Raw File Name)=11_FFA_D2O_BT474_Control.raw; RAW_FILE_NAME(Raw File Name)=NEG_11_FFA_D2O_BT474_Control.mzXML; RAW_FILE_NAME(Raw File Name )=POS_11_FFA_D2O_BT474_Control.mzXML SUBJECT_SAMPLE_FACTORS - 12_FFA_D2O_BT474_GSK0001 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 nM GSK2194069 RAW_FILE_NAME(Raw File Name)=12_FFA_D2O_BT474_GSK0001.raw; RAW_FILE_NAME(Raw File Name)=NEG_12_FFA_D2O_BT474_GSK0001.mzXML; RAW_FILE_NAME(Raw File Name )=POS_12_FFA_D2O_BT474_GSK0001.mzXML SUBJECT_SAMPLE_FACTORS - 13_FFA_D2O_BT474_GSK0040 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 nM GSK2194069 RAW_FILE_NAME(Raw File Name)=13_FFA_D2O_BT474_GSK0040.raw; RAW_FILE_NAME(Raw File Name)=NEG_13_FFA_D2O_BT474_GSK0040.mzXML; RAW_FILE_NAME(Raw File Name )=POS_13_FFA_D2O_BT474_GSK0040.mzXML SUBJECT_SAMPLE_FACTORS - 14_FFA_D2O_BT474_GSK1000 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM GSK2194069 RAW_FILE_NAME(Raw File Name)=14_FFA_D2O_BT474_GSK1000.raw; RAW_FILE_NAME(Raw File Name)=NEG_14_FFA_D2O_BT474_GSK1000.mzXML; RAW_FILE_NAME(Raw File Name )=POS_14_FFA_D2O_BT474_GSK1000.mzXML SUBJECT_SAMPLE_FACTORS - 15_FFA_D2O_BT474_Fasnall01 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM Fasnall RAW_FILE_NAME(Raw File Name)=15_FFA_D2O_BT474_Fasnall01.raw; RAW_FILE_NAME(Raw File Name)=NEG_15_FFA_D2O_BT474_Fasnall01.mzXML; RAW_FILE_NAME(Raw File Name )=POS_15_FFA_D2O_BT474_Fasnall01.mzXML SUBJECT_SAMPLE_FACTORS - 16_FFA_D2O_BT474_Fasnall05 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:5 uM Fasnall RAW_FILE_NAME(Raw File Name)=16_FFA_D2O_BT474_Fasnall05.raw; RAW_FILE_NAME(Raw File Name)=NEG_16_FFA_D2O_BT474_Fasnall05.mzXML; RAW_FILE_NAME(Raw File Name )=POS_16_FFA_D2O_BT474_Fasnall05.mzXML SUBJECT_SAMPLE_FACTORS - 17_FFA_D2O_BT474_Fasnall40 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 uM Fasnall RAW_FILE_NAME(Raw File Name)=17_FFA_D2O_BT474_Fasnall40.raw; RAW_FILE_NAME(Raw File Name)=NEG_17_FFA_D2O_BT474_Fasnall40.mzXML; RAW_FILE_NAME(Raw File Name )=POS_17_FFA_D2O_BT474_Fasnall40.mzXML SUBJECT_SAMPLE_FACTORS - 18_FFA_D2O_BT474_Control Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:Vehicle RAW_FILE_NAME(Raw File Name)=18_FFA_D2O_BT474_Control.raw; RAW_FILE_NAME(Raw File Name)=NEG_18_FFA_D2O_BT474_Control.mzXML; RAW_FILE_NAME(Raw File Name )=POS_18_FFA_D2O_BT474_Control.mzXML SUBJECT_SAMPLE_FACTORS - 19_FFA_D2O_BT474_GSK0001 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 nM GSK2194069 RAW_FILE_NAME(Raw File Name)=19_FFA_D2O_BT474_GSK0001.raw; RAW_FILE_NAME(Raw File Name)=NEG_19_FFA_D2O_BT474_GSK0001.mzXML; RAW_FILE_NAME(Raw File Name )=POS_19_FFA_D2O_BT474_GSK0001.mzXML SUBJECT_SAMPLE_FACTORS - 20_FFA_D2O_BT474_GSK0040 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 nM GSK2194069 RAW_FILE_NAME(Raw File Name)=20_FFA_D2O_BT474_GSK0040.raw; RAW_FILE_NAME(Raw File Name)=NEG_20_FFA_D2O_BT474_GSK0040.mzXML; RAW_FILE_NAME(Raw File Name )=POS_20_FFA_D2O_BT474_GSK0040.mzXML SUBJECT_SAMPLE_FACTORS - 21_FFA_D2O_BT474_GSK1000 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM GSK2194069 RAW_FILE_NAME(Raw File Name)=21_FFA_D2O_BT474_GSK1000.raw; RAW_FILE_NAME(Raw File Name)=NEG_21_FFA_D2O_BT474_GSK1000.mzXML; RAW_FILE_NAME(Raw File Name )=POS_21_FFA_D2O_BT474_GSK1000.mzXML SUBJECT_SAMPLE_FACTORS - 22_FFA_D2O_BT474_Fasnall01 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM Fasnall RAW_FILE_NAME(Raw File Name)=22_FFA_D2O_BT474_Fasnall01.raw; RAW_FILE_NAME(Raw File Name)=NEG_22_FFA_D2O_BT474_Fasnall01.mzXML; RAW_FILE_NAME(Raw File Name )=POS_22_FFA_D2O_BT474_Fasnall01.mzXML SUBJECT_SAMPLE_FACTORS - 23_FFA_D2O_BT474_Fasnall05 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:5 uM Fasnall RAW_FILE_NAME(Raw File Name)=23_FFA_D2O_BT474_Fasnall05.raw; RAW_FILE_NAME(Raw File Name)=NEG_23_FFA_D2O_BT474_Fasnall05.mzXML; RAW_FILE_NAME(Raw File Name )=POS_23_FFA_D2O_BT474_Fasnall05.mzXML SUBJECT_SAMPLE_FACTORS - 24_FFA_D2O_BT474_Fasnall40 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 uM Fasnall RAW_FILE_NAME(Raw File Name)=24_FFA_D2O_BT474_Fasnall40.raw; RAW_FILE_NAME(Raw File Name)=NEG_24_FFA_D2O_BT474_Fasnall40.mzXML; RAW_FILE_NAME(Raw File Name )=POS_24_FFA_D2O_BT474_Fasnall40.mzXML SUBJECT_SAMPLE_FACTORS - 25_FFA_Blank Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA RAW_FILE_NAME(Raw File Name)=25_FFA_Blank.raw; RAW_FILE_NAME(Raw File Name)=NEG_25_FFA_Blank.mzXML; RAW_FILE_NAME(Raw File Name )=POS_25_FFA_Blank.mzXML SUBJECT_SAMPLE_FACTORS - 26_FFA_Blank Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA RAW_FILE_NAME(Raw File Name)=26_FFA_Blank.raw; RAW_FILE_NAME(Raw File Name)=NEG_26_FFA_Blank.mzXML; RAW_FILE_NAME(Raw File Name )=POS_26_FFA_Blank.mzXML SUBJECT_SAMPLE_FACTORS - 27_FFA_Blank Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA RAW_FILE_NAME(Raw File Name)=27_FFA_Blank.raw; RAW_FILE_NAME(Raw File Name)=NEG_27_FFA_Blank.mzXML; RAW_FILE_NAME(Raw File Name )=POS_27_FFA_Blank.mzXML #COLLECTION CO:COLLECTION_SUMMARY Cells were seeded in 10 cm Petri dishes. At collection, cells were washed with CO:COLLECTION_SUMMARY PBS three times. Then, 1 ml of methanol was added and cells were scraped from CO:COLLECTION_SUMMARY the surface. All content of the plate was transferred into 13 x 100 mm Pyrex CO:COLLECTION_SUMMARY glass tubes. Lipids were extracted by the Folch method. Dried lipids were CO:COLLECTION_SUMMARY redissolved in 1 ml of 0.3 M KOH solution in 90% methanol and incubated at 85 CO:COLLECTION_SUMMARY °C for 1 h. Then, 100 µl of formic acid were added, followed by 800 µl of CO:COLLECTION_SUMMARY hexane for extraction. The hexane phase was transferred to glass LC-MS vials and CO:COLLECTION_SUMMARY dried under the stream of nitrogen. Samples were redissolved in 1 ml of 1:1 CO:COLLECTION_SUMMARY methanol:isopropanol. CO:COLLECTION_PROTOCOL_FILENAME DM_free_fatty_acid_analysis_samples.txt CO:SAMPLE_TYPE Cultured cells CO:COLLECTION_METHOD 100% methanol extraction CO:VOLUMEORAMOUNT_COLLECTED 1 ml CO:STORAGE_CONDITIONS -80℃ CO:COLLECTION_VIALS 1.5 ml plastic centrifuge tubes CO:STORAGE_VIALS 1.5 ml plastic centrifuge tubes #TREATMENT TR:TREATMENT_SUMMARY Cells were grown in 20% D2O-containing RPMI-1640 medium and treated with Fasnall TR:TREATMENT_SUMMARY or GSK2194069 at various concentrations. TR:TREATMENT_COMPOUND Fasnall, GSK2194069 TR:TREATMENT_DOSE 1 nM - 40 uM TR:TREATMENT_DOSEDURATION 24 h TR:TREATMENT_VEHICLE DMSO TR:CELL_GROWTH_CONTAINER 6-cm Petri dishes TR:CELL_MEDIA RPMI-1640 TR:CELL_ENVIR_COND 37C, 5% CO2 TR:CELL_PCT_CONFLUENCE ~70% #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Sample preparation for LC-MS free fatty acid analysis Cells were seeded in 10 cm SP:SAMPLEPREP_SUMMARY Petri dishes. At collection, cells were washed with PBS three times. Then, 1 ml SP:SAMPLEPREP_SUMMARY of methanol was added and cells were scraped from the surface. All content of SP:SAMPLEPREP_SUMMARY the plate was transferred into 13 x 100 mm Pyrex glass tubes. Lipids were SP:SAMPLEPREP_SUMMARY extracted by the Folch method. Dried lipids were redissolved in 1 ml of 0.3 M SP:SAMPLEPREP_SUMMARY KOH solution in 90% methanol and incubated at 85 °C for 1 h. Then, 100 µl of SP:SAMPLEPREP_SUMMARY formic acid were added, followed by 800 µl of hexane for extraction. The hexane SP:SAMPLEPREP_SUMMARY phase was transferred to glass LC-MS vials and dried under the stream of SP:SAMPLEPREP_SUMMARY nitrogen. Samples were redissolved in 1 ml of 1:1 methanol:isopropanol. SP:SAMPLEPREP_PROTOCOL_FILENAME DM_free_fatty_acid_analysis_samples.txt SP:PROCESSING_METHOD Lipid saponification in 0.3 M KOH SP:EXTRACTION_METHOD 100% methanol SP:EXTRACT_ENRICHMENT None SP:EXTRACT_CLEANUP None SP:EXTRACT_STORAGE -80℃ SP:SAMPLE_RESUSPENSION None SP:SAMPLE_DERIVATIZATION None SP:SAMPLE_SPIKING None SP:SUBCELLULAR_LOCATION Cellular lipids #CHROMATOGRAPHY CH:CHROMATOGRAPHY_TYPE Reversed phase CH:INSTRUMENT_NAME Thermo Dionex Ultimate 3000 RS CH:COLUMN_NAME Phenomenex Kinetex XB-C18 (150 x 3 mm, 2.6 um) CH:SOLVENT_A 60:40 Acetonitrile/water; 10 mM ammonium formate CH:SOLVENT_B 90:8:2 Isopropanol/acetonitrile/water; 10 mM ammonium formate CH:FLOW_GRADIENT 0-4.5 min, 15-60% B; 4.5-12 min, 60-82% B; 12-12.75 min, 82-95% B; 12.75-16.5 CH:FLOW_GRADIENT min, 95-100% B; 16.5-22.5 min, 100% B; 22.5-22.6 min, 100-15% B; 22.6-25 min, CH:FLOW_GRADIENT 15% B CH:FLOW_RATE 0-22.5 min, 0.333 ml/min; 22.5-22.6 min, 0.333-0.5 ml/min; 22.6-24.9 min, 0.5 CH:FLOW_RATE ml/min; 24.9-25 min, 0.5-0.333 ml/min CH:COLUMN_TEMPERATURE 65 CH:INJECTION_TEMPERATURE 20 #ANALYSIS AN:ANALYSIS_TYPE MS AN:LABORATORY_NAME Wistar Institute Proteomics & Metabolomic Core AN:OPERATOR_NAME Dzmitry Mukha AN:DETECTOR_TYPE Orbitrap #MS MS:INSTRUMENT_NAME Thermo Q Exactive HF-X Orbitrap MS:INSTRUMENT_TYPE Orbitrap MS:MS_TYPE ESI MS:ION_MODE POSITIVE MS:MS_COMMENTS The HESI ion source voltage was set to the following parameters: +3,300/-3,500 MS:MS_COMMENTS V, sheath gas 50, auxiliary gas 20, spare gas 0, probe heater 350 °C, capillary MS:MS_COMMENTS temperature 350 °C, S-Lens RF level 80. The mass spectrometer was set to MS:MS_COMMENTS acquire data in polarity-switching mode, one microscan, 60,000 resolution, AGC MS:MS_COMMENTS target 5e6, scan range 130-1950 m/z, IT 200 ms. Data were converted into the MS:MS_COMMENTS mzXML format by ProteoWizard and analyzed in MAVEN. Free cholesterol was MS:MS_COMMENTS measured as a water-loss in-source fragment [M-H2O+H]+. MS:CAPILLARY_TEMPERATURE 350 MS:ION_SOURCE_TEMPERATURE 350 MS:ION_SPRAY_VOLTAGE 3300 MS:IONIZATION Both MS:SOURCE_TEMPERATURE 350 MS:AUTOMATIC_GAIN_CONTROL 5e6 MS:DATAFORMAT RAW #MS_METABOLITE_DATA MS_METABOLITE_DATA:UNITS AU MS_METABOLITE_DATA_START Samples 01_FFA_Blank 02_FFA_Blank 03_FFA_Blank 04_FFA_D2O_BT474_Control 05_FFA_D2O_BT474_GSK0001 06_FFA_D2O_BT474_GSK0040 07_FFA_D2O_BT474_GSK1000 08_FFA_D2O_BT474_Fasnall01 09_FFA_D2O_BT474_Fasnall05 10_FFA_D2O_BT474_Fasnall40 11_FFA_D2O_BT474_Control 12_FFA_D2O_BT474_GSK0001 13_FFA_D2O_BT474_GSK0040 14_FFA_D2O_BT474_GSK1000 15_FFA_D2O_BT474_Fasnall01 16_FFA_D2O_BT474_Fasnall05 17_FFA_D2O_BT474_Fasnall40 18_FFA_D2O_BT474_Control 19_FFA_D2O_BT474_GSK0001 20_FFA_D2O_BT474_GSK0040 21_FFA_D2O_BT474_GSK1000 22_FFA_D2O_BT474_Fasnall01 23_FFA_D2O_BT474_Fasnall05 24_FFA_D2O_BT474_Fasnall40 25_FFA_Blank 26_FFA_Blank 27_FFA_Blank Factors Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:Vehicle Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 nM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 nM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:5 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:Vehicle Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 nM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 nM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:5 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:Vehicle Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 nM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 nM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM GSK2194069 Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:1 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:5 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:20% D2O | Drug Treatment:40 uM Fasnall Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA Sample source:BT-474 cell lipid extract | Isotopic Tracer:NA | Drug Treatment:NA Cholesterol [M-H2O+H]+ C12 PARENT 219599.3 0 0 3.76E+07 3.31E+07 2.89E+07 2.93E+07 3.47E+07 3.40E+07 3.20E+07 3.48E+07 3.72E+07 3.45E+07 3.22E+07 3.37E+07 3.58E+07 2.82E+07 3.84E+07 3.55E+07 3.54E+07 3.32E+07 3.58E+07 3.27E+07 3.29E+07 0 0 0 Cholesterol [M-H2O+H]+ D-label-1 0 0 0 1461776 0 957827.6 0 1107391 0 0 0 0 1344681 3624670 0 0 3248171 0 2771207 0 0 0 1016960 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-3 0 0 0 686256.8 558953 566677.4 261738.5 189877.1 0 0 463400 596418.3 500893.9 222997.2 48249.73 0 0 644784.9 358254.1 491191.2 156446.7 122504 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-4 0 0 0 735378.8 757760.8 554551.3 373458.5 164870.1 0 0 592720.7 554694.9 596485.7 336700.8 131206.9 0 0 766578.2 621389.9 483282.4 322978.2 143735.9 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-5 0 0 0 692097.6 615402.6 577390.8 408962 0 0 0 609620.3 596673.2 629561.3 457038.9 0 0 0 734367 624043.6 523758.5 298584.2 78852.22 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-6 0 0 0 426119.1 377336.4 358373.4 214659 55350.31 0 0 443308.8 348883.4 294487.3 236783 46024.92 0 0 501254.6 339079.7 426032 206776.3 40728.71 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-7 0 0 0 269157.9 212773.9 203311.5 137529.2 46256.77 0 0 278165.8 205565.3 242193.7 174173.3 15728.8 0 0 314394.8 261387.9 199616.6 109320 43001.59 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-8 0 0 0 120342.1 104220.4 70812.5 95681.99 0 0 0 148832.1 81070.76 90043 83404.91 0 0 0 143828.6 123071.9 76485.27 58079.84 14782.26 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-9 0 0 0 17746.07 0 37507.07 0 0 0 0 39280.68 17922.64 17333.82 0 0 0 0 33246.61 16096.32 18425.38 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-10 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-11 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-12 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-13 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-14 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-15 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-16 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-17 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-18 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-19 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-20 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-21 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-22 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-23 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-24 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-25 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-26 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-27 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-28 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-29 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-30 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-31 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-32 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-33 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-34 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-35 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-36 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-37 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-38 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-39 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-40 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-41 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-42 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-43 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Cholesterol [M-H2O+H]+ D-label-44 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 MS_METABOLITE_DATA_END #METABOLITES METABOLITES_START metabolite_name retention time quantified m/z parent pubchem id kegg id regno comments Cholesterol [M-H2O+H]+ C12 PARENT 9.813006 369.3522 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-1 9.802023 370.3566 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-2 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-3 9.790095 372.3711 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-4 9.788138 373.377 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-5 9.786216 374.3819 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-6 9.783252 375.3893 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-7 9.777384 376.3953 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-8 9.779448 377.4012 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-9 9.77599 378.4075 369.3522 5997 C00187 34361 Cholesterol [M-H2O+H]+ D-label-10 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-11 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-12 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-13 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-14 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-15 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-16 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-17 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-18 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-19 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-20 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-21 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-22 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-23 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-24 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-25 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-26 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-27 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-28 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-29 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-30 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-31 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-32 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-33 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-34 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-35 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-36 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-37 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-38 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-39 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-40 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-41 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-42 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-43 NA NA 369.3522 5997 C00187 34361 Peak was not detected Cholesterol [M-H2O+H]+ D-label-44 NA NA 369.3522 5997 C00187 34361 Peak was not detected METABOLITES_END #END