#METABOLOMICS WORKBENCH rushingb_20240716_130949 DATATRACK_ID:5009 STUDY_ID:ST003370 ANALYSIS_ID:AN005522 PROJECT_ID:PR002092 VERSION 1 CREATED_ON July 26, 2024, 6:42 am #PROJECT PR:PROJECT_TITLE An untargeted metabolomic analysis of acute AFB1 treatment in liver, breast, and PR:PROJECT_TITLE lung cells PR:PROJECT_SUMMARY Aflatoxin B1 (AFB1) is a class 1 carcinogen and mycotoxin known to contribute to PR:PROJECT_SUMMARY the development of hepatocellular carcinoma (HCC), growth impairment, altered PR:PROJECT_SUMMARY immune system modulation, and malnutrition. AFB1 is synthesized by Aspergillus PR:PROJECT_SUMMARY flavus and is known to widely contaminate foodstuffs, particularly maize, wheat, PR:PROJECT_SUMMARY and groundnuts. The mechanism in which AFB1 causes genetic mutations has been PR:PROJECT_SUMMARY well studied, however its metabolomic effects remained largely unknown. A better PR:PROJECT_SUMMARY understanding of how AFB1 disrupts metabolism would provide insight into how PR:PROJECT_SUMMARY this mycotoxin leads to carcinogenesis, growth impairment, and/or PR:PROJECT_SUMMARY immunomodulation, and may reveal potential targets for pharmacological or PR:PROJECT_SUMMARY nutritional interventions to protect against these effects. The current study PR:PROJECT_SUMMARY evaluated the metabolomic effects of various doses (2.5 µM, 5 µM, 10uM) of PR:PROJECT_SUMMARY AFB1 treatment to HepG2 (liver), MDA-MB-231 (breast), and A549 (lung) cells. PR:PROJECT_SUMMARY Treated and control cells’ metabolomic profiles were evaluated via ultra-high PR:PROJECT_SUMMARY performance liquid chromatography-high resolution mass spectrometry PR:PROJECT_SUMMARY (UHPLC-HRMS). Univariate and multivariate analyses revealed significant PR:PROJECT_SUMMARY alterations in metabolite concentrations from each dose of AFB1 treatment in PR:PROJECT_SUMMARY each cell type. Pathway analysis was then used to understand broader biochemical PR:PROJECT_SUMMARY functions affected by AFB1 treatment in each cell type. HepG2 cell pathway PR:PROJECT_SUMMARY analyses revealed significant pathway perturbations in lipid metabolism, PR:PROJECT_SUMMARY carnitine synthesis, catecholamine biosynthesis, purine metabolism, and PR:PROJECT_SUMMARY spermidine and spermine biosynthesis. Analysis of A549 cells found a greater PR:PROJECT_SUMMARY emphasis of perturbations on various amino acids along with lipid PR:PROJECT_SUMMARY synthesis-related pathways, and catecholamine biosynthesis. Finally, analysis of PR:PROJECT_SUMMARY treated MDA-MB-231 cells found spermidine and spermine biosynthesis, carnitine PR:PROJECT_SUMMARY synthesis, plasma membrane-related pathways (phosphatidylcholine synthesis and PR:PROJECT_SUMMARY alpha linolenic acid and linoleic acid metabolism), and various amino acid PR:PROJECT_SUMMARY metabolism pathways to be most affected. These highlighted pathways should be PR:PROJECT_SUMMARY targeted in future investigations to evaluate their potential in mitigating or PR:PROJECT_SUMMARY preventing the development of negative health effects associated with AFB1 PR:PROJECT_SUMMARY exposure. PR:INSTITUTE UNC-Chapel Hill PR:LAST_NAME Rushing PR:FIRST_NAME Blake PR:ADDRESS 500 Laureate Way, Kannapolis, NC, 28081, USA PR:EMAIL blake_rushing@unc.edu PR:PHONE +1 (704) 250-5000 #STUDY ST:STUDY_TITLE An untargeted metabolomic analysis of acute AFB1 treatment in liver, breast, and ST:STUDY_TITLE lung cells ST:STUDY_SUMMARY Aflatoxin B1 (AFB1) is a class 1 carcinogen and mycotoxin known to contribute to ST:STUDY_SUMMARY the development of hepatocellular carcinoma (HCC), growth impairment, altered ST:STUDY_SUMMARY immune system modulation, and malnutrition. AFB1 is synthesized by Aspergillus ST:STUDY_SUMMARY flavus and is known to widely contaminate foodstuffs, particularly maize, wheat, ST:STUDY_SUMMARY and groundnuts. The mechanism in which AFB1 causes genetic mutations has been ST:STUDY_SUMMARY well studied, however its metabolomic effects remained largely unknown. A better ST:STUDY_SUMMARY understanding of how AFB1 disrupts metabolism would provide insight into how ST:STUDY_SUMMARY this mycotoxin leads to carcinogenesis, growth impairment, and/or ST:STUDY_SUMMARY immunomodulation, and may reveal potential targets for pharmacological or ST:STUDY_SUMMARY nutritional interventions to protect against these effects. The current study ST:STUDY_SUMMARY evaluated the metabolomic effects of various doses (2.5 µM, 5 µM, 10uM) of ST:STUDY_SUMMARY AFB1 treatment to HepG2 (liver), MDA-MB-231 (breast), and A549 (lung) cells. ST:STUDY_SUMMARY Treated and control cells’ metabolomic profiles were evaluated via ultra-high ST:STUDY_SUMMARY performance liquid chromatography-high resolution mass spectrometry ST:STUDY_SUMMARY (UHPLC-HRMS). Univariate and multivariate analyses revealed significant ST:STUDY_SUMMARY alterations in metabolite concentrations from each dose of AFB1 treatment in ST:STUDY_SUMMARY each cell type. Pathway analysis was then used to understand broader biochemical ST:STUDY_SUMMARY functions affected by AFB1 treatment in each cell type. HepG2 cell pathway ST:STUDY_SUMMARY analyses revealed significant pathway perturbations in lipid metabolism, ST:STUDY_SUMMARY carnitine synthesis, catecholamine biosynthesis, purine metabolism, and ST:STUDY_SUMMARY spermidine and spermine biosynthesis. Analysis of A549 cells found a greater ST:STUDY_SUMMARY emphasis of perturbations on various amino acids along with lipid ST:STUDY_SUMMARY synthesis-related pathways, and catecholamine biosynthesis. Finally, analysis of ST:STUDY_SUMMARY treated MDA-MB-231 cells found spermidine and spermine biosynthesis, carnitine ST:STUDY_SUMMARY synthesis, plasma membrane-related pathways (phosphatidylcholine synthesis and ST:STUDY_SUMMARY alpha linolenic acid and linoleic acid metabolism), and various amino acid ST:STUDY_SUMMARY metabolism pathways to be most affected. These highlighted pathways should be ST:STUDY_SUMMARY targeted in future investigations to evaluate their potential in mitigating or ST:STUDY_SUMMARY preventing the development of negative health effects associated with AFB1 ST:STUDY_SUMMARY exposure. ST:INSTITUTE UNC-Chapel Hill ST:LAST_NAME Rushing ST:FIRST_NAME Blake ST:ADDRESS 500 Laureate Way ST:EMAIL blake_rushing@unc.edu ST:PHONE 7042505000 #SUBJECT SU:SUBJECT_TYPE Cultured cells SU:SUBJECT_SPECIES Homo sapiens SU:TAXONOMY_ID 9606 #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 - B_1_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_1_A549_AFB1 SUBJECT_SAMPLE_FACTORS - B_1_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_1_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - B_1_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_1_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - B_2_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_2_A549_AFB1 SUBJECT_SAMPLE_FACTORS - B_2_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_2_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - B_2_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_2_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - B_3_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_3_A549_AFB1 SUBJECT_SAMPLE_FACTORS - B_3_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_3_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - B_3_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_3_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - B_4_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_4_A549_AFB1 SUBJECT_SAMPLE_FACTORS - B_4_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_4_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - B_4_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):- | Sample source:blank RAW_FILE_NAME=B_4_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_1_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_1_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_1_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_1_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_1_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_1_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_10_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_10_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_10_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_10_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_10_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_10_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_11_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_11_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_11_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_11_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_11_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_11_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_12_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_12_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_12_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_12_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_12_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_12_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_13_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_13_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_13_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_13_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_13_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_13_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_14_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_14_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_14_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_14_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_14_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_14_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_15_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_15_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_15_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_15_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_15_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_15_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_16_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_16_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_16_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_16_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_16_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_16_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_2_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_2_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_2_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_2_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_2_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_2_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_3_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_3_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_3_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_3_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_3_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_3_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_4_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_4_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_4_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_4_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_4_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_4_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_5_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_5_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_5_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_5_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_5_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_5_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_6_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_6_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_6_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_6_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_6_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):2.5 | Sample source:Cultured cells RAW_FILE_NAME=S_6_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_7_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_7_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_7_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_7_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_7_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):5 | Sample source:Cultured cells RAW_FILE_NAME=S_7_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_8_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_8_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_8_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_8_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_8_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):10 | Sample source:Cultured cells RAW_FILE_NAME=S_8_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - S_9_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_9_A549_AFB1 SUBJECT_SAMPLE_FACTORS - S_9_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_9_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - S_9_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):0 | Sample source:Cultured cells RAW_FILE_NAME=S_9_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - SP_1_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_1_A549_AFB1 SUBJECT_SAMPLE_FACTORS - SP_1_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_1_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - SP_1_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_1_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - SP_2_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_2_A549_AFB1 SUBJECT_SAMPLE_FACTORS - SP_2_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_2_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - SP_2_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_2_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - SP_3_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_3_A549_AFB1 SUBJECT_SAMPLE_FACTORS - SP_3_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_3_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - SP_3_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_3_MDAMB231_AFB1 SUBJECT_SAMPLE_FACTORS - SP_4_A549_AFB1 cell line:A549 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_4_A549_AFB1 SUBJECT_SAMPLE_FACTORS - SP_4_HepG2_AFB1 cell line:HepG2 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_4_HepG2_AFB1 SUBJECT_SAMPLE_FACTORS - SP_4_MDAMB231_AFB1 cell line:MDA-MB-231 | AFB1 dose (micromolar):- | Sample source:pooled sample RAW_FILE_NAME=SP_4_MDAMB231_AFB1 #COLLECTION CO:COLLECTION_SUMMARY Briefly, treatment media was aspirated, and cells were washed with 2 mL of CO:COLLECTION_SUMMARY ice-cold PBS followed by the addition of 1 mL of an ice-cold solution of 80% CO:COLLECTION_SUMMARY methanol and 20% water. Cells were detached using cell scrapers and vortexed at CO:COLLECTION_SUMMARY 5000 rpm for 10 min. Protein concentration was measured by a bicinchoninic acid CO:COLLECTION_SUMMARY (BCA) assay, and additional 80% methanol was added to each tube to normalize for CO:COLLECTION_SUMMARY protein concentration. Samples were centrifuged at 16,000× g at 4 °C for 10 CO:COLLECTION_SUMMARY min and supernatants were transferred to autosampler vials for analysis by CO:COLLECTION_SUMMARY ultra-high-pressure liquid chromatography–high-resolution mass spectrometry CO:COLLECTION_SUMMARY (UHPLC-HRMS). Quality control study pools (QCSP) were created by combining 50 CO:COLLECTION_SUMMARY µL of each sample into a single mixture. Three separate QCSPs were made for CO:COLLECTION_SUMMARY each cell line. Method blanks were created by adding 500 µL of 80% methanol to CO:COLLECTION_SUMMARY empty tubes and were processed in an identical manner as the study samples. All CO:COLLECTION_SUMMARY samples for a given cell line were derived from the same cryovial. CO:SAMPLE_TYPE Cultured cells #TREATMENT TR:TREATMENT_SUMMARY A549, HepG2, and MDA-MB-231 cells were cultured in DMEM supplemented with 10% TR:TREATMENT_SUMMARY FBS, 2 mM glutamine, 50 U/mL penicillin, and 50 µg/mL streptomycin. Cells were TR:TREATMENT_SUMMARY plated in 6 well plates and grown to 80% confluency and were treated with AFB1 TR:TREATMENT_SUMMARY at doses of 0, 2.5, 5, and 10 µM. Dimethyl sulfoxide (DMSO) was used as the TR:TREATMENT_SUMMARY vehicle with a concentration of 0.1% for all treatments. All treatments were TR:TREATMENT_SUMMARY performed for 24 h (n=4 per treatment). #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Cells were washed three times with ice cold PBS, then quenched with 1 volume of SP:SAMPLEPREP_SUMMARY -20°C cold Acetonitrile (Fisher, A955-1) and collected with additional 0.75 SP:SAMPLEPREP_SUMMARY volume of ultra-pure H2O (Pierce, PI51140). All sample groups included SP:SAMPLEPREP_SUMMARY biological triplicates. Spheroid extracts were dried by speed vac overnight and SP:SAMPLEPREP_SUMMARY then reconstituted in a volume of 95:5 water:methanol that was proportional to SP:SAMPLEPREP_SUMMARY each sample’s protein concentration. Samples were vortexed for 10 min at 5000 SP:SAMPLEPREP_SUMMARY rpm and then centrifuged for 10 min at 16000 x g at 4°C. Supernatants were SP:SAMPLEPREP_SUMMARY transferred to autosampler vials and an aliquot of 10 mL was taken from each SP:SAMPLEPREP_SUMMARY sample and combined into a single mixture to make a quality control study pool SP:SAMPLEPREP_SUMMARY (QCSP). LC-MS grade water was processed in an identical manner as the study SP:SAMPLEPREP_SUMMARY samples to prepare method blanks. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_TYPE Reversed phase CH:INSTRUMENT_NAME Thermo Vanquish CH:COLUMN_NAME Waters ACQUITY UPLC HSS T3 (100 x 2.1mm,1.8um) CH:SOLVENT_A 100% water; 0.1% formic acid CH:SOLVENT_B 100% methanol; 0.1% formic acid CH:FLOW_GRADIENT 0 min, 1% B; 1 min, 1% B; 16 min, 99% B; 19 min, 99%B; 19.5 min, 1% B; 22 min, CH:FLOW_GRADIENT 1%B CH:FLOW_RATE 0.4 mL/min CH:COLUMN_TEMPERATURE 50 ℃ #ANALYSIS AN:ANALYSIS_TYPE MS #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 Metabolomics data were acquired on a Vanquish UHPLC system coupled to a Q MS:MS_COMMENTS Exactive™ HF-X Hybrid Quadrupole-Orbitrap Mass Spectrometer (Thermo Fisher MS:MS_COMMENTS Scientific, San Jose, CA). Metabolites were separated via an HSS T3 C18 column MS:MS_COMMENTS (2.1 × 100 mm, 1.7 µm, Waters Corporation) at 50 °C with binary mobile MS:MS_COMMENTS phase of water (A) and methanol (B), each containing 0.1% formic acid (v/v). The MS:MS_COMMENTS UHPLC linear gradient started from 2% B, and increased to 100% B in 16 min, then MS:MS_COMMENTS held for 4 min, with the flow rate at 400 µL/min. The untargeted data was MS:MS_COMMENTS acquired from 70 to 1050 m/z using the data-dependent acquisition mode. Method MS:MS_COMMENTS blanks and SP injections were placed after every 6 samples (n=3 each). MS:MS_COMMENTS Progenesis QI (version 2.1, Waters Corporation) was used for peak picking, MS:MS_COMMENTS alignment, and normalization. Background signals were filtered out by removing MS:MS_COMMENTS peaks with a fold change less than 3 in the total SP vs the blank injections. MS:MS_COMMENTS Samples were then normalized in Progenesis QI using the “normalize to all” MS:MS_COMMENTS feature. Filtered, normalized data was exported and multivariate analysis was MS:MS_COMMENTS performed using SIMCA 16. MS:MS_RESULTS_FILE ST003370_AN005522_Results.txt UNITS:Normalized data. All data is unitless. Note that masses ending in "m/z" are mass-to-charge values while those ending in "n" are neutral masses Has m/z:Yes Has RT:Yes RT units:Minutes #END