#METABOLOMICS WORKBENCH dk3039_20231205_020157 DATATRACK_ID:4488 STUDY_ID:ST002999 ANALYSIS_ID:AN004926 PROJECT_ID:PR001869 VERSION 1 CREATED_ON December 7, 2023, 9:55 am #PROJECT PR:PROJECT_TITLE Metabolic Reprogramming by Histone Deacetylase Inhibition Preferentially Targets PR:PROJECT_TITLE NRF2-activated tumors PR:PROJECT_SUMMARY Interplay between metabolism and chromatin signaling are implicated in cancer PR:PROJECT_SUMMARY progression. However, whether and how metabolic reprogramming in tumors PR:PROJECT_SUMMARY generates chromatin vulnerabilities remain unclear. Lung adenocarcinoma (LUAD) PR:PROJECT_SUMMARY tumors frequently harbor aberrant activation of the NRF2 antioxidant pathway PR:PROJECT_SUMMARY which drives aggressive and chemo-resistant disease. Using a chromatin-focused PR:PROJECT_SUMMARY CRISPR screen we report that NRF2 activation sensitizes LUAD cells to genetic PR:PROJECT_SUMMARY and chemical inhibition of class I histone deacetylases (HDAC). This association PR:PROJECT_SUMMARY is observed across cultured cells, mouse models and patient-derived xenografts. PR:PROJECT_SUMMARY Integrative epigenomic, transcriptomic and metabolomic analysis demonstrates PR:PROJECT_SUMMARY that HDAC inhibition causes widespread redistribution of H4ac and its reader PR:PROJECT_SUMMARY protein, which transcriptionally downregulates metabolic enzymes. This results PR:PROJECT_SUMMARY in reduced flux into amino acid metabolism and de novo nucleotide synthesis PR:PROJECT_SUMMARY pathways that are preferentially required for the survival of NRF2-active cancer PR:PROJECT_SUMMARY cells. Together, our findings suggest NRF2 activation as a potential biomarker PR:PROJECT_SUMMARY for effective repurposing of HDAC inhibitors to treat solid tumors. PR:INSTITUTE Columbia University Medical Center PR:DEPARTMENT Genetics and Development PR:LABORATORY Chao Lu PR:LAST_NAME Karagiannis PR:FIRST_NAME Dimitris PR:ADDRESS 630 West 168th Street, NEW YORK, NY, 10032, USA PR:EMAIL karagiannis_dimitrios@yahoo.gr PR:PHONE +30 6982804931 #STUDY ST:STUDY_TITLE Metabolomics and glucose and glutamine labeled isotope tracing analysis in ST:STUDY_TITLE murine lung adenocarcinoma cells in the context of normal or active NRF2 pathway ST:STUDY_TITLE as well as HDAC and glutaminase inhibitor treatment. ST:STUDY_SUMMARY Interplay between metabolism and chromatin signaling are implicated in cancer ST:STUDY_SUMMARY progression. However, whether and how metabolic reprogramming in tumors ST:STUDY_SUMMARY generates chromatin vulnerabilities remain unclear. Lung adenocarcinoma (LUAD) ST:STUDY_SUMMARY tumors frequently harbor aberrant activation of the NRF2 antioxidant pathway ST:STUDY_SUMMARY which drives aggressive and chemo-resistant disease. Using a chromatin-focused ST:STUDY_SUMMARY CRISPR screen we report that NRF2 activation sensitizes LUAD cells to genetic ST:STUDY_SUMMARY and chemical inhibition of class I histone deacetylases (HDAC). This association ST:STUDY_SUMMARY is observed across cultured cells, mouse models and patient-derived xenografts. ST:STUDY_SUMMARY Integrative epigenomic, transcriptomic and metabolomic analysis demonstrates ST:STUDY_SUMMARY that HDAC inhibition causes widespread redistribution of H4ac and its reader ST:STUDY_SUMMARY protein, which transcriptionally downregulates metabolic enzymes. This results ST:STUDY_SUMMARY in reduced flux into amino acid metabolism and de novo nucleotide synthesis ST:STUDY_SUMMARY pathways that are preferentially required for the survival of NRF2-active cancer ST:STUDY_SUMMARY cells. Together, our findings suggest NRF2 activation as a potential biomarker ST:STUDY_SUMMARY for effective repurposing of HDAC inhibitors to treat solid tumors. In this ST:STUDY_SUMMARY metabolomics experiment we characterize the changes in metabolic pathway flux in ST:STUDY_SUMMARY KP LUAD cells in response to HDAC and glutaminase inhibition. This dataset ST:STUDY_SUMMARY includes metabolomics of U-C13 glucose tracing (1h and 24h) and U-C13 glutamine ST:STUDY_SUMMARY (8h) of mouse LUAD cell lines with Kras overexpression and p53 knock-out (KP), ST:STUDY_SUMMARY carrying empty vector (EV) or overexpression of NRF2dNeh2 (NRF2) and treated ST:STUDY_SUMMARY with DMSO, Romidepsin or CB-839. 3 technical replicates were done per condition ST:STUDY_SUMMARY in 2 separate experiments, 1: glucose tracing and 2: glutamine tracing. ST:INSTITUTE Columbia University - Medical Center ST:DEPARTMENT Genetics and Development ST:LABORATORY Chao Lu ST:LAST_NAME Dimitris ST:FIRST_NAME Karagiannis ST:ADDRESS 622 W 168th St, New York, NY 10032 ST:EMAIL karagiannis_dimitrios@yahoo.gr ST:PHONE +30 6982804931 #SUBJECT SU:SUBJECT_TYPE Cultured cells SU:SUBJECT_SPECIES Mus musculus SU:TAXONOMY_ID 10090 #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 NA blank1 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=blank1.mzML SUBJECT_SAMPLE_FACTORS NA blank2 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=blank2.mzML SUBJECT_SAMPLE_FACTORS NA blank3 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=blank3.mzML SUBJECT_SAMPLE_FACTORS NA blank4 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=blank4.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_CB839_Gln_1 Genotype:Empty vector | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_CB839_Gln_1.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_CB839_Gln_2 Genotype:Empty vector | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_CB839_Gln_2.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_CB839_Gln_3 Genotype:Empty vector | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_CB839_Gln_3.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_1h_1 Genotype:Empty vector | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_DMSO_1h_1.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_1h_2 Genotype:Empty vector | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_DMSO_1h_2.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_1h_3 Genotype:Empty vector | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_DMSO_1h_3.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_24h_1 Genotype:Empty vector | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_DMSO_24h_1.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_24h_2 Genotype:Empty vector | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_DMSO_24h_2.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_24h_3 Genotype:Empty vector | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_DMSO_24h_3.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_Gln_1 Genotype:Empty vector | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_DMSO_Gln_1.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_Gln_2 Genotype:Empty vector | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_DMSO_Gln_2.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_DMSO_Gln_3 Genotype:Empty vector | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_DMSO_Gln_3.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_Rom_1h_1 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_Rom_1h_1.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_Rom_1h_2 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_Rom_1h_2.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_Rom_1h_3 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_Rom_1h_3.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_Rom_24h_1 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_Rom_24h_1.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_Rom_24h_2 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_Rom_24h_2.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_Rom_24h_3 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=EV_Rom_24h_3.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_ROM_Gln_1 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_ROM_Gln_1.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_ROM_Gln_2 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_ROM_Gln_2.mzML SUBJECT_SAMPLE_FACTORS KP_EV EV_ROM_Gln_3 Genotype:Empty vector | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=EV_ROM_Gln_3.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_CB839_Gln_1 Genotype:NRF2 overexpression | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_CB839_Gln_1.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_CB839_Gln_2 Genotype:NRF2 overexpression | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_CB839_Gln_2.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_CB839_Gln_3 Genotype:NRF2 overexpression | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_CB839_Gln_3.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_1h_1 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_DMSO_1h_1.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_1h_2 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_DMSO_1h_2.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_1h_3 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_DMSO_1h_3.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_24h_1 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_DMSO_24h_1.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_24h_2 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_DMSO_24h_2.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_24h_3 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_DMSO_24h_3.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_Gln_1 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_DMSO_Gln_1.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_Gln_2 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_DMSO_Gln_2.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_DMSO_Gln_3 Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_DMSO_Gln_3.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_Rom_1h_1 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_Rom_1h_1.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_Rom_1h_2 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_Rom_1h_2.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_Rom_1h_3 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_Rom_1h_3.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_Rom_24h_1 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_Rom_24h_1.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_Rom_24h_2 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_Rom_24h_2.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_Rom_24h_3 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Experiment=1_20211110; RAW_FILE_NAME=NRF2_Rom_24h_3.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_ROM_Gln_1 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_ROM_Gln_1.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_ROM_Gln_2 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_ROM_Gln_2.mzML SUBJECT_SAMPLE_FACTORS KP_NRF2 NRF2_ROM_Gln_3 Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Experiment=2_20220428; RAW_FILE_NAME=NRF2_ROM_Gln_3.mzML SUBJECT_SAMPLE_FACTORS NA QC_1 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=2_20220428; RAW_FILE_NAME=QC_1.mzML SUBJECT_SAMPLE_FACTORS NA QC_2 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=2_20220428; RAW_FILE_NAME=QC_2.mzML SUBJECT_SAMPLE_FACTORS NA QC_3 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=2_20220428; RAW_FILE_NAME=QC_3.mzML SUBJECT_SAMPLE_FACTORS NA QC_4 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=2_20220428; RAW_FILE_NAME=QC_4.mzML SUBJECT_SAMPLE_FACTORS NA QC1 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=QC1.mzML SUBJECT_SAMPLE_FACTORS NA QC2 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=QC2.mzML SUBJECT_SAMPLE_FACTORS NA QC3 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=QC3.mzML SUBJECT_SAMPLE_FACTORS NA QC4 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=QC4.mzML SUBJECT_SAMPLE_FACTORS NA QC5 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=1_20211110; RAW_FILE_NAME=QC5.mzML SUBJECT_SAMPLE_FACTORS NA Blank_1 Genotype:NA | Treatment:NA | Timepoint:NA | Tracer:NA Experiment=2_20220428; RAW_FILE_NAME=Blank_1.mzML #COLLECTION CO:COLLECTION_SUMMARY Mouse lung adenocarcinoma (LUAD) cell lines were established as in a previous CO:COLLECTION_SUMMARY study by the Papagiannakopoulos lab (Romero et al. Nature Medicine 2017). CO:COLLECTION_SUMMARY Briefly, KrasLSL-G12D/+; p53flox/flox genetically engineered mice were CO:COLLECTION_SUMMARY intratracheally infected with pSECC lentiviral vectors expressing sgRNAs against CO:COLLECTION_SUMMARY Keap1 or tdTomato as a control. The mice developed LUAD tumors and cell lines CO:COLLECTION_SUMMARY were derived from them. In this experiment we used a cell line derived from CO:COLLECTION_SUMMARY control tumors (KP: Kras-mutant, p53-null). In this cell line we overexpressed CO:COLLECTION_SUMMARY an active form of NRF2 (NRF2) or introduced the empty vector (EV). CO:SAMPLE_TYPE Cultured cells #TREATMENT TR:TREATMENT_SUMMARY For glucose tracing analysis, 2x105 KP cells (n=3) were plated in 6-well plates TR:TREATMENT_SUMMARY overnight in RPMI medium (Sigma). After 24 hours, the media was replaced with TR:TREATMENT_SUMMARY fresh RPMI medium containing DMSO or Romidepsin. At 48 hours the media was TR:TREATMENT_SUMMARY replaced with fresh glucose-free RPMI medium (Sigma) containing 10% dialyzed TR:TREATMENT_SUMMARY fetal bovine serum (Gibco), 2.0 g/L 13C6-glucose (Sigma) and DMSO or 5nM TR:TREATMENT_SUMMARY Romidepsin. Cells were harvested at 49 and 72 hours and processed as described TR:TREATMENT_SUMMARY below. For glutamine tracing, 2x105 KP cells (n=3) were plated in 6-well plates TR:TREATMENT_SUMMARY overnight in RPMI medium (Sigma). After 24 hours, the media was replaced with TR:TREATMENT_SUMMARY fresh RPMI medium containing DMSO, 1nM Romidepsin or 150nM CB-839. At 48 hours TR:TREATMENT_SUMMARY the media was replaced with fresh glutamine-free RPMI medium (Sigma) containing TR:TREATMENT_SUMMARY 10% dialyzed fetal bovine serum (Gibco), 2.0 g/L 13C6-glutamine (Cambridge TR:TREATMENT_SUMMARY Isotope Laboratories) and DMSO, 1nM Romidepsin or 150nM CB-839 #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Cells were washed with cold PBS, lysed in 80% Ultra LC-MS acetonitrile (Thermo SP:SAMPLEPREP_SUMMARY Scientific) supplemented with 20 µM deuterated 2-hydroxyglutarate SP:SAMPLEPREP_SUMMARY (D-2-hydroxyglutaric-2,3,3,4,4-d5 acid (d5-2HG), Cambridge Isotope Laboratories) SP:SAMPLEPREP_SUMMARY as an internal standard on ice for 15 minutes, and centrifuged for 10 minutes at SP:SAMPLEPREP_SUMMARY 20,000 x g at 4 °C. 200 µL of supernatants were subjected to mass spectrometry SP:SAMPLEPREP_SUMMARY analysis. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_TYPE HILIC CH:INSTRUMENT_NAME Agilent 1290 Infinity CH:COLUMN_NAME Merck SeQuant ZIC-HILIC (150 x 2.1mm,5um) CH:SOLVENT_A 25 mM ammonium carbonate in water CH:SOLVENT_B acetonitrile CH:FLOW_GRADIENT 0-1.5 min, 80% B; 1.5-7 min, 80% B to 50% B, 7-8.5 min, 50% B; 8.5-8.7 min, 50% CH:FLOW_GRADIENT B to 80% B, 8.7-13 min, 80% B CH:FLOW_RATE 0.3 mL/min CH:COLUMN_TEMPERATURE 35 #ANALYSIS AN:ANALYSIS_TYPE MS #MS MS:INSTRUMENT_NAME Agilent 6545 QTOF MS:INSTRUMENT_TYPE QTOF MS:MS_TYPE ESI MS:ION_MODE NEGATIVE MS:MS_COMMENTS The overall runtime was 13 minutes, and the injection volume was 5 µL. The MS:MS_COMMENTS Agilent Q-TOF was operated in negative mode and the relevant parameters were as MS:MS_COMMENTS listed: ion spray voltage, 3500 V; nozzle voltage, 1000 V; fragmentor voltage, MS:MS_COMMENTS 125 V; drying gas flow, 11 L/min; capillary temperature, 325 °C; drying gas MS:MS_COMMENTS temperature, 350 °C; and nebulizer pressure, 40 psi. A full scan range was set MS:MS_COMMENTS at 50 to 1600 (m/z). The reference masses were 119.0363 and 980.0164. The MS:MS_COMMENTS acquisition rate was 2 spectra/s. Targeted analysis, isotopologues extraction MS:MS_COMMENTS (for the metabolic tracing study), and natural isotope abundance correction were MS:MS_COMMENTS performed by the Agilent Profinder B.10.00 Software (Agilent Technologies). #MS_METABOLITE_DATA MS_METABOLITE_DATA:UNITS Abundance (Extracted ion chromatogram core area) MS_METABOLITE_DATA_START Samples EV_DMSO_1h_1 EV_DMSO_1h_2 EV_DMSO_1h_3 EV_DMSO_24h_1 EV_DMSO_24h_2 EV_DMSO_24h_3 EV_Rom_1h_1 EV_Rom_1h_2 EV_Rom_1h_3 EV_Rom_24h_1 EV_Rom_24h_2 EV_Rom_24h_3 NRF2_DMSO_1h_1 NRF2_DMSO_1h_2 NRF2_DMSO_1h_3 NRF2_DMSO_24h_1 NRF2_DMSO_24h_2 NRF2_DMSO_24h_3 NRF2_Rom_1h_1 NRF2_Rom_1h_2 NRF2_Rom_1h_3 NRF2_Rom_24h_1 NRF2_Rom_24h_2 NRF2_Rom_24h_3 EV_DMSO_Gln_1 NRF2_DMSO_Gln_2 NRF2_ROM_Gln_2 NRF2_CB839_Gln_2 EV_DMSO_Gln_3 EV_ROM_Gln_3 EV_CB839_Gln_3 NRF2_DMSO_Gln_3 NRF2_ROM_Gln_3 NRF2_CB839_Gln_3 EV_ROM_Gln_1 EV_CB839_Gln_1 NRF2_DMSO_Gln_1 NRF2_ROM_Gln_1 NRF2_CB839_Gln_1 EV_DMSO_Gln_2 EV_ROM_Gln_2 EV_CB839_Gln_2 Factors Genotype:Empty vector | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:1 hour | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:24 hours | Tracer:U-C13 Glucose Genotype:Empty vector | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:Empty vector | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:Empty vector | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:Empty vector | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:Empty vector | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:Empty vector | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:NRF2 overexpression | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:Empty vector | Treatment:DMSO | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:Empty vector | Treatment:Romidepsin | Timepoint:8 hours | Tracer:U-C13 Glutamine Genotype:Empty vector | Treatment:CB-839 | Timepoint:8 hours | Tracer:U-C13 Glutamine Citric acid 9703905 10039190 9652787 8420485 6811671 4818766 6808011 7691035 5227506 8053279 5772542 4342688 3889894 7875880 4962037 7117551 10829799 10436017 6232296 4985864 4194055 11887838 7853048 7718016 12885419 257312556 141140527 208661898 43477044 22275043 119551134 251083503 205948538 164621532 78314898 69337020 111780432 171547484 194973395 112768460 76179663 226479367 L-Glutamate 27580302 34924121 42269286 20403174 24189441 23169393 21178370 16109699 18053176 10563561 10977803 10672864 42826057 26932363 41977337 29386744 23991138 23300901 14757804 17017996 17816602 9739633 12721216 9670175 39152359 46612569 22722229 8609921 30513774 9129717 11353092 47533420 26605608 11196291 21197592 11440457 32438715 23102962 8204356 44307632 22645190 10922776 Fumaric acid 642596 1709828 104030 1317369 4428931 6804722 1794772 551730 1185672 1425147 2014536 2198168 5774811 652261 5812514 5782279 4714044 5621889 1611579 2275146 3199192 2030483 5137740 3923433 14075758 11131200 9322436 6678911 11641135 4493464 7118564 11476304 11248255 5632047 13433437 6299782 7820186 9723789 5822880 15622235 13743383 9599693 L-Malic acid 3913594 10642969 12890667 7336755 27663119 43445675 10687873 5719968 7301193 13512797 12365603 16772018 36184458 4027600 36673395 35630793 29011455 34719814 9631199 13737965 19532159 12052406 31913230 24739320 109088072 82557008 69526076 46824585 24572 30547 22837 84558619 86210019 38447792 33688 31260 56384809 7770 39460415 119394474 31843 68248699 Succinic acid 407875 1422455 852042 421880 800136 1440530 185115 105048 519157 406838 335430 331316 1360502 161437 1203175 1185709 721214 1264793 430900 485047 553542 557299 528968 487259 1597227 2460234 1133449 1588093 1343245 259970 1138781 2998654 1761766 1389822 1088730 840976 1180991 1268274 1473839 2247608 1007333 1819938 Oxoglutaric acid 199673 295422 346119 97615 161455 193479 321356 122868 218548 105339 143696 180263 302716 174103 324775 189807 141360 156321 116651 140220 125161 100478 167928 105455 245622 77055 429023 38210 554193 273248 49735 134180 242528 29335 444540 26325 57649 91219 37674 349536 678960 33751 Pyruvate 489856 298172 615141 657208 179892 103606 54821 96016 68874 65392 52552 35636 328110 544544 268335 301731 213165 123067 122762 141394 138917 124923 108432 80489 636689 1510292 1145225 184651 828377 318621 334714 1952020 1201095 453953 270525 356075 1504387 1047664 193099 560887 383137 213887 Uridine triphosphate (UTP) 2911005 6924621 9750239 3858198 7154539 7280015 3807056 1577897 2945001 2666096 2603648 2389098 10184891 3577607 10804949 7828739 5931815 6292197 3343093 3876284 4983912 2918176 4569828 3543491 6889865 2035183 882649 1519069 1053194 0 787451 1691383 1641694 1252310 1089288 618912 958075 907314 1346420 9519081 716843 4004845 Adenosine triphosphate (ATP) 3678369 6257982 8276401 5510498 7364648 8318932 4853018 2493014 3845170 3505903 3750675 3459381 9770730 4247836 9580605 9668827 7527519 7740248 4108880 4788171 5744060 3806198 5816213 4693883 12079107 9652165 3335399 4833439 3521621 371716 3267167 6708823 5630610 3394128 5185846 3013594 4025183 3512965 4040674 16035117 5082101 10267957 L-Lactic acid 1946456 3297617 4174776 17001197 6098693 5815201 865522 877521 1165572 2838265 1236981 1168822 3036472 3444470 3897287 13628433 12189742 10936151 1336141 1416869 1426377 4928059 3976615 3595176 7691051 11334385 2891500 5880207 8618764 1029898 7829069 17558543 3387568 8925523 2117346 5976271 11299610 3907286 6847800 7455194 1463890 6700648 L-Serine 889786 715881 655647 783442 537733 581583 698695 1006549 915777 1231198 1059878 1142206 906402 1023761 1020077 390501 390650 318251 668718 606318 569865 700623 578473 641631 3563555 4523773 3938506 3017024 2470788 1481760 2592042 4689678 5565337 2636979 3694906 2451136 3049999 4498432 2929148 4201648 3654164 4011151 D-Glyceraldehyde 3-phosphate 858244 1417326 1497022 840583 1345582 2798547 2379558 923864 1893131 817670 1068142 1361819 3382849 1150765 3932061 4546297 2445008 3208523 2466562 3189516 4073610 1529885 3320734 2491184 1236388 4574771 816393 3830392 1428032 85860 2664605 4471471 1505219 3224025 288779 1850966 1900182 710281 2473425 2540416 352980 4450000 D-Glycerate 3-phosphate 762198 475130 946732 668163 2618382 5914696 2118407 625663 1654717 1460226 1801425 2092514 2108396 740883 3997815 6862568 5654822 5865637 1266563 2366357 4545001 2218395 4616142 3727382 2293608 7382590 2532055 4508962 1998889 339350 3127777 6201416 3447689 3541502 2141944 3116629 4136849 3339555 4307548 3840600 2233782 5157699 D-Glucose 6-phosphate 168324 343370 405874 139116 182370 231204 381752 204168 364481 156021 174839 185392 663468 275180 723576 332683 234737 297755 395581 488859 545685 209420 307887 234702 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Guanosine triphosphate (GTP) 156263 331977 477581 220075 337378 352511 215954 102308 158734 128978 122859 99061 490300 182931 520143 463800 373620 386397 199924 207882 284404 169111 259983 198333 422673 691423 229757 521037 245500 51870 415412 558039 364302 345334 284478 349392 289973 290969 457730 697032 256306 970948 L-Glutamine NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 12830452 18362521 16345281 63330202 6726325 4797556 44739765 15587779 21171916 56525455 13201020 40368680 14644411 19885154 59531398 11767287 12154844 66452150 MS_METABOLITE_DATA_END #METABOLITES METABOLITES_START metabolite_name PubChem KEGG Tgt RT Expected m/z Citric acid 311 C00158 12.5 191.0197 L-Glutamate 33032 C00025 7.55 NA Fumaric acid 444972 C00122 9 115.0037 L-Malic acid 222656 C00149 9 NA Succinic acid 1110 C00042 7 117.0193 Oxoglutaric acid 51 C00026 7.2 145.01373 Pyruvate 1060 C00022 1.5 87.00088 Uridine triphosphate (UTP) 6133 C00075 12.6 NA Adenosine triphosphate (ATP) 5957 C00002 12.5 505.9885 L-Lactic acid 107689 C00186 2.44 89.0244 L-Serine 5951 C00065 7.6 NA D-Glyceraldehyde 3-phosphate 3418 C00118 10.873 NA D-Glycerate 3-phosphate 439183 C00197 11 NA D-Glucose 6-phosphate 5958 C00092 11.5 NA Guanosine triphosphate (GTP) 6830 C00044 13.5 521.9834 L-Glutamine 5961 C00064 8.44 145.0619 METABOLITES_END #END