#METABOLOMICS WORKBENCH Brodesser_20230816_054636 DATATRACK_ID:4224 STUDY_ID:ST003114 ANALYSIS_ID:AN005103 PROJECT_ID:PR001935 VERSION 1 CREATED_ON March 6, 2024, 10:51 am #PROJECT PR:PROJECT_TITLE Lipid unsaturation promotes BAX and BAK pore activity during apoptosis PR:PROJECT_SUMMARY BAX and BAK are proapoptotic members of the BCL2 family that directly mediate PR:PROJECT_SUMMARY mitochondrial outer membrane permeabilization (MOMP), a central step in PR:PROJECT_SUMMARY apoptosis execution. However, the molecular architecture of the mitochondrial PR:PROJECT_SUMMARY apoptotic pore remains a key open question and especially little is known about PR:PROJECT_SUMMARY the contribution of lipids to MOMP. By performing a comparative lipidomics PR:PROJECT_SUMMARY analysis of the proximal membrane environment of BAK isolated in lipid PR:PROJECT_SUMMARY nanodiscs, we find a significant enrichment of unsaturated species nearby BAK PR:PROJECT_SUMMARY and BAX in apoptotic conditions. We then demonstrate that unsaturated lipids PR:PROJECT_SUMMARY promote BAX pore activity in model membranes, isolated mitochondria and cellular PR:PROJECT_SUMMARY systems, which is further supported by molecular dynamics simulations. PR:PROJECT_SUMMARY Accordingly, the fatty acid desaturase FADS2 not only enhances apoptosis PR:PROJECT_SUMMARY sensitivity, but also the activation of the cGAS/STING pathway downstream mtDNA PR:PROJECT_SUMMARY release. The correlation of FADS2 levels with the sensitization to apoptosis of PR:PROJECT_SUMMARY different lung and kidney cancer cell lines by co-treatment with unsaturated PR:PROJECT_SUMMARY fatty acids supports the relevance of our findings. Altogether, our work PR:PROJECT_SUMMARY provides new insight on how local lipid environment affects BAX and BAK function PR:PROJECT_SUMMARY during apoptosis. PR:INSTITUTE University of Cologne PR:DEPARTMENT Institute for Genetics, Cluster of Excellence Cellular Stress Responses in PR:DEPARTMENT Aging-associated Diseases (CECAD) PR:LAST_NAME García-Sáez PR:FIRST_NAME Ana J. PR:ADDRESS Joseph-Stelzmann-Str. 26, 50931 Cologne, Germany PR:EMAIL ana.garcia@uni-koeln.de PR:PHONE +49 221 478 84261 PR:CONTRIBUTORS Shashank Dadsena, Rodrigo Cuevas Arenas, Gonçalo Vieira, Susanne Brodesser, PR:CONTRIBUTORS Manuel N. Melo, Ana J. García-Sáez #STUDY ST:STUDY_TITLE Lipidomics analyses in model membranes, isolated mitochondria and cellular ST:STUDY_TITLE systems to study how the local lipid environment affects BAX and BAK function ST:STUDY_TITLE during apoptosis. ST:STUDY_SUMMARY To investigate how the local lipid environment affects BAX and BAK function ST:STUDY_SUMMARY during apoptosis, we performed quantitative analyses of different lipid classes ST:STUDY_SUMMARY (glycerophospholipids, fatty acids, ceramides and sphingomyelins) in cultured ST:STUDY_SUMMARY cells, isolated mitochondria and lipid nanodics formed by Styrene-Malic Acid ST:STUDY_SUMMARY (SMA) co-polymers. Ceramides, sphingomyelins, fatty acids and cardiolipins were ST:STUDY_SUMMARY analyzed by Liquid Chromatography coupled to Tandem Mass Spectrometry ST:STUDY_SUMMARY (LC-MS/MS). For glycerophospholipids (PC, PE, PI, PS, PG, PA) we applied direct ST:STUDY_SUMMARY infusion MS approaches (Shotgun Lipidomics). ST:INSTITUTE University of Cologne ST:DEPARTMENT Faculty of Medicine and University Hospital of Cologne, Cluster of Excellence ST:DEPARTMENT Cellular Stress Responses in Aging-associated Diseases (CECAD) ST:LABORATORY CECAD Lipidomics/Metabolomics Facility ST:LAST_NAME Brodesser ST:FIRST_NAME Susanne ST:ADDRESS Joseph-Stelzmann-Str. 26, 50931 Cologne, Germany ST:EMAIL susanne.brodesser@uk-koeln.de ST:PHONE +49 221 478 84015 #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 - S01_mitos_control.SMA_1 Sample source:mitochondrial SMALPs | Genotype:WT | Condition:control RAW_FILE_NAME=GPL_S01_mitos_control.SMA_1.mzML; RAW_FILE_NAME=CerSM_S01_mitos_control.SMA_1.mzML; RAW_FILE_NAME=CL_S01_mitos_control.SMA_1.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S02_mitos_control.SMA_2 Sample source:mitochondrial SMALPs | Genotype:WT | Condition:control RAW_FILE_NAME=GPL_S02_mitos_control.SMA_2.mzML; RAW_FILE_NAME=CerSM_S02_mitos_control.SMA_2.mzML; RAW_FILE_NAME=CL_S02_mitos_control.SMA_2.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S03_mitos_control.SMA_3 Sample source:mitochondrial SMALPs | Genotype:WT | Condition:control RAW_FILE_NAME=-; RAW_FILE_NAME=CerSM_S03_mitos_control.SMA_3.mzML; RAW_FILE_NAME=CL_S03_mitos_control.SMA_3.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S04_mitos_control.SMA_4 Sample source:mitochondrial SMALPs | Genotype:WT | Condition:control RAW_FILE_NAME=GPL_S04_mitos_control.SMA_4.mzML; RAW_FILE_NAME=CerSM_S04_mitos_control.SMA_4.mzML; RAW_FILE_NAME=CL_S04_mitos_control.SMA_4.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S05_mitos_apoptosis.SMA_1 Sample source:mitochondrial SMALPs | Genotype:WT | Condition:apoptotic RAW_FILE_NAME=GPL_S05_mitos_apoptosis.SMA_1.mzML; RAW_FILE_NAME=CerSM_S05_mitos_apoptosis.SMA_1.mzML; RAW_FILE_NAME=CL_S05_mitos_apoptosis.SMA_1.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S06_mitos_apoptosis.SMA_2 Sample source:mitochondrial SMALPs | Genotype:WT | Condition:apoptotic RAW_FILE_NAME=GPL_S06_mitos_apoptosis.SMA_2.mzML; RAW_FILE_NAME=CerSM_S06_mitos_apoptosis.SMA_2.mzML; RAW_FILE_NAME=CL_S06_mitos_apoptosis.SMA_2.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S07_mitos_apoptosis.SMA_3 Sample source:mitochondrial SMALPs | Genotype:WT | Condition:apoptotic RAW_FILE_NAME=GPL_S07_mitos_apoptosis.SMA_3.mzML; RAW_FILE_NAME=CerSM_S07_mitos_apoptosis.SMA_3.mzML; RAW_FILE_NAME=CL_S07_mitos_apoptosis.SMA_3.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S08_mitos_apoptosis.SMA_4 Sample source:mitochondrial SMALPs | Genotype:WT | Condition:apoptotic RAW_FILE_NAME=-; RAW_FILE_NAME=CerSM_S08_mitos_apoptosis.SMA_4.mzML; RAW_FILE_NAME=CL_S08_mitos_apoptosis.SMA_4.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S09_mitos_control_1 Sample source:total mitochondria | Genotype:WT | Condition:control RAW_FILE_NAME=GPL_S09_mitos_control_1.mzML; RAW_FILE_NAME=CerSM_S09_mitos_control_1.mzML; RAW_FILE_NAME=CL_S09_mitos_control_1.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S10_mitos_control_2 Sample source:total mitochondria | Genotype:WT | Condition:control RAW_FILE_NAME=-; RAW_FILE_NAME=CerSM_S10_mitos_control_2.mzML; RAW_FILE_NAME=CL_S10_mitos_control_2.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S11_mitos_control_3 Sample source:total mitochondria | Genotype:WT | Condition:control RAW_FILE_NAME=GPL_S11_mitos_control_3.mzML; RAW_FILE_NAME=CerSM_S11_mitos_control_3.mzML; RAW_FILE_NAME=CL_S11_mitos_control_3.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S12_mitos_control_4 Sample source:total mitochondria | Genotype:WT | Condition:control RAW_FILE_NAME=GPL_S12_mitos_control_4.mzML; RAW_FILE_NAME=CerSM_S12_mitos_control_4.mzML; RAW_FILE_NAME=CL_S12_mitos_control_4.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S13_mitos_apoptosis_1 Sample source:total mitochondria | Genotype:WT | Condition:apoptotic RAW_FILE_NAME=GPL_S13_mitos_apoptosis_1.mzML; RAW_FILE_NAME=CerSM_S13_mitos_apoptosis_1.mzML; RAW_FILE_NAME=CL_S13_mitos_apoptosis_1.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S14_mitos_apoptosis_2 Sample source:total mitochondria | Genotype:WT | Condition:apoptotic RAW_FILE_NAME=-; RAW_FILE_NAME=CerSM_S14_mitos_apoptosis_2.mzML; RAW_FILE_NAME=CL_S14_mitos_apoptosis_2.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S15_mitos_apoptosis_3 Sample source:total mitochondria | Genotype:WT | Condition:apoptotic RAW_FILE_NAME=GPL_S15_mitos_apoptosis_3.mzML; RAW_FILE_NAME=CerSM_S15_mitos_apoptosis_3.mzML; RAW_FILE_NAME=CL_S15_mitos_apoptosis_3.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S16_mitos_apoptosis_4 Sample source:total mitochondria | Genotype:WT | Condition:apoptotic RAW_FILE_NAME=GPL_S16_mitos_apoptosis_4.mzML; RAW_FILE_NAME=CerSM_S16_mitos_apoptosis_4.mzML; RAW_FILE_NAME=CL_S16_mitos_apoptosis_4.mzML; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S02_pulldown_Control_22.08 Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:control RAW_FILE_NAME=GPL_S02_pulldown_Control_22.08.mzML; RAW_FILE_NAME=CerSM_S02_pulldown_Control_22.08.mzML; RAW_FILE_NAME=-; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S03_pulldown_Control_01.09 Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:control RAW_FILE_NAME=GPL_S03_pulldown_Control_01.09.mzML; RAW_FILE_NAME=CerSM_S03_pulldown_Control_01.09.mzML; RAW_FILE_NAME=-; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S04_pulldown_Control_04.09 Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:control RAW_FILE_NAME=GPL_S04_pulldown_Control_04.09.mzML; RAW_FILE_NAME=CerSM_S04_pulldown_Control_04.09.mzML; RAW_FILE_NAME=-; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S05_pulldown_Control_31.09 Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:control RAW_FILE_NAME=GPL_S05_pulldown_Control_31.09.mzML; RAW_FILE_NAME=CerSM_S05_pulldown_Control_31.09.mzML; RAW_FILE_NAME=-; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S06_pulldown_Apoptosis_22.08 Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:apoptotic RAW_FILE_NAME=GPL_S06_pulldown_Apoptosis_22.08.mzML; RAW_FILE_NAME=CerSM_S06_pulldown_Apoptosis_22.08.mzML; RAW_FILE_NAME=-; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S07_pulldown_Apoptosis_01.09 Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:apoptotic RAW_FILE_NAME=GPL_S07_pulldown_Apoptosis_01.09.mzML; RAW_FILE_NAME=CerSM_S07_pulldown_Apoptosis_01.09.mzML; RAW_FILE_NAME=-; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S08_pulldown_Apoptosis_04.09 Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:apoptotic RAW_FILE_NAME=GPL_S08_pulldown_Apoptosis_04.09.mzML; RAW_FILE_NAME=CerSM_S08_pulldown_Apoptosis_04.09.mzML; RAW_FILE_NAME=-; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S09_pulldown_Apoptosis_31.09 Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:apoptotic RAW_FILE_NAME=GPL_S09_pulldown_Apoptosis_31.09.mzML; RAW_FILE_NAME=CerSM_S09_pulldown_Apoptosis_31.09.mzML; RAW_FILE_NAME=-; RAW_FILE_NAME=- SUBJECT_SAMPLE_FACTORS - S01_mitos_no.treatment_WT_1 Sample source:total mitochondria | Genotype:WT | Condition:untreated RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S01_mitos_no.treatment_WT_1.mzML SUBJECT_SAMPLE_FACTORS - S02_mitos_no.treatment_WT_2 Sample source:total mitochondria | Genotype:WT | Condition:untreated RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S02_mitos_no.treatment_WT_2.mzML SUBJECT_SAMPLE_FACTORS - S03_mitos_no.treatment_WT_3 Sample source:total mitochondria | Genotype:WT | Condition:untreated RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S03_mitos_no.treatment_WT_3.mzML SUBJECT_SAMPLE_FACTORS - S04_mitos_no.treatment_WT_4 Sample source:total mitochondria | Genotype:WT | Condition:untreated RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S04_mitos_no.treatment_WT_4.mzML SUBJECT_SAMPLE_FACTORS - S05_mitos_linoleic.acid_WT_1 Sample source:total mitochondria | Genotype:WT | Condition:linoleic acid RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S05_mitos_linoleic.acid_WT_1.mzML SUBJECT_SAMPLE_FACTORS - S06_mitos_linoleic.acid_WT_2 Sample source:total mitochondria | Genotype:WT | Condition:linoleic acid RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S06_mitos_linoleic.acid_WT_2.mzML SUBJECT_SAMPLE_FACTORS - S07_mitos_linoleic.acid_WT_3 Sample source:total mitochondria | Genotype:WT | Condition:linoleic acid RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S07_mitos_linoleic.acid_WT_3.mzML SUBJECT_SAMPLE_FACTORS - S08_mitos_linoleic.acid_WT_4 Sample source:total mitochondria | Genotype:WT | Condition:linoleic acid RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S08_mitos_linoleic.acid_WT_4.mzML SUBJECT_SAMPLE_FACTORS - S09_smitos_no.treatment_KO_1 Sample source:total mitochondria | Genotype:FADS2 KO | Condition:untreated RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S09_mitos_no.treatment_KO_1.mzML SUBJECT_SAMPLE_FACTORS - S10_mitos_no.treatment_KO_2 Sample source:total mitochondria | Genotype:FADS2 KO | Condition:untreated RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S10_mitos_no.treatment_KO_2.mzML SUBJECT_SAMPLE_FACTORS - S11_mitos_no.treatment_KO_3 Sample source:total mitochondria | Genotype:FADS2 KO | Condition:untreated RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S11_mitos_no.treatment_KO_3.mzML SUBJECT_SAMPLE_FACTORS - S12_mitos_no.treatment_KO_4 Sample source:total mitochondria | Genotype:FADS2 KO | Condition:untreated RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S12_mitos_no.treatment_KO_4.mzML SUBJECT_SAMPLE_FACTORS - S13_mitos_linoleic.acid_KO_1 Sample source:total mitochondria | Genotype:FADS2 KO | Condition:linoleic acid RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S13_mitos_linoleic.acid_KO_1.mzML SUBJECT_SAMPLE_FACTORS - S14_mitos_linoleic.acid_KO_2 Sample source:total mitochondria | Genotype:FADS2 KO | Condition:linoleic acid RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S14_mitos_linoleic.acid_KO_2.mzML SUBJECT_SAMPLE_FACTORS - S15_mitos_linoleic.acid_KO_3 Sample source:total mitochondria | Genotype:FADS2 KO | Condition:linoleic acid RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S15_mitos_linoleic.acid_KO_3.mzML SUBJECT_SAMPLE_FACTORS - S16_mitos_linoleic.acid_KO_4 Sample source:total mitochondria | Genotype:FADS2 KO | Condition:linoleic acid RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=-; RAW_FILE_NAME=FA_S16_mitos_linoleic.acid_KO_4.mzML #COLLECTION CO:COLLECTION_SUMMARY Human osteosarcoma U2OS WT, U2OS BAK Ko expressing GFP BAK, and U2OS FADS2 KO CO:COLLECTION_SUMMARY cell lines were cultured at 37 °C and 5% CO2 in DMEM supplemented with 10% FBS CO:COLLECTION_SUMMARY and 1% penicillin/streptomycin (Invitrogen, Germany). For lipidomic experiments CO:COLLECTION_SUMMARY cells were incubated with 1 μM of ABT-737 and S63845 in the complete media and CO:COLLECTION_SUMMARY incubated for 50 min at 37°C and 5% CO2. FADS2 KO in U2OS cells was generated CO:COLLECTION_SUMMARY in the lab by the CRISPR/Cas9 method. Linoleic acid stock (50 mM) was prepared CO:COLLECTION_SUMMARY in ethanol and diluted into culture media before adding them to the cells. CO:COLLECTION_SUMMARY Mitochondria were isolated from cultured human osteosarcoma cells by mechanical CO:COLLECTION_SUMMARY disruption of cells followed by differential centrifugation: Cells were CO:COLLECTION_SUMMARY harvested by trypsinization, washed in PBS, and then resuspend in isolation CO:COLLECTION_SUMMARY buffer (IM;250 mM sucrose, 5 mM Tris, and 2 mM EDTA; pH 7.4 and protease CO:COLLECTION_SUMMARY inhibitor cocktail) and mechanically broken using glass homogenizer on ice CO:COLLECTION_SUMMARY (30-40 strokes on ice) and total cellular lysates were spin down first to remove CO:COLLECTION_SUMMARY nuclei and cell debris at 600 x g for 5 min and later at 10,800 x g for 10 min CO:COLLECTION_SUMMARY at 4°C to get the crude mitochondria. Mitochondrial pellet was washed 2-3 times CO:COLLECTION_SUMMARY with isolation buffer to remove other impurities from mitochondria. Isolated CO:COLLECTION_SUMMARY mitochondria were solubilized using SMA co-polymer. For this, mitochondria CO:COLLECTION_SUMMARY either from apoptotic or healthy cells were incubated with 0.5% SMA (2:1) for 45 CO:COLLECTION_SUMMARY min at room temperature with gentle rotation. Mitochondrial membrane was spun CO:COLLECTION_SUMMARY down at 100,000 x g for 40 min to separate solubilized SMALP from the CO:COLLECTION_SUMMARY insolubilized membrane. Next, the size of SMALP was analyzed by Dynamic Light CO:COLLECTION_SUMMARY Scattering (DLS). For DLS measurements, 15 μl of sample was added to a quartz CO:COLLECTION_SUMMARY cuvette which had been thoroughly cleaned with Milli-Q H2O. The cuvette was CO:COLLECTION_SUMMARY placed in DynaPro NanoStar (Wyatt Technology corporation, USA) and the sample CO:COLLECTION_SUMMARY was analyzed using 10 runs with 10 second acquisition time. This helps to CO:COLLECTION_SUMMARY determine the mass distribution of the sample as well as the estimated size of CO:COLLECTION_SUMMARY the particles. The distance distribution is shown on a log scale. The size of CO:COLLECTION_SUMMARY SMALP as well as the homogeneity with in the sample were also checked by CO:COLLECTION_SUMMARY Negative Transmission Electron Microscopy (TEM). For this the diluted SMALPs CO:COLLECTION_SUMMARY were placed onto a glow-discharged copper grid (Electron Microscopy Sciences) CO:COLLECTION_SUMMARY coated with a layer of thin carbon, washed twice with water, stained with 2% CO:COLLECTION_SUMMARY uranyl acetate for 5 min and then air-dried. The grids were imaged on a JEOL CO:COLLECTION_SUMMARY JEM2100PLUS electron microscope and recorded with a GATAN OneView camera (CECAD CO:COLLECTION_SUMMARY Imaging Facility). mEGFP-BAK-SMALPs were affinity purified from total CO:COLLECTION_SUMMARY solubilized mitochondrial membrane fraction (SMALP). For this total SMALP were CO:COLLECTION_SUMMARY incubated with 25 μl of GFP-trap MA beads for 90 min with slow rotation in cold CO:COLLECTION_SUMMARY room. Beads were washed 2 times with 100 μl of Tris buffer (50 mM Tris 150 mM CO:COLLECTION_SUMMARY NaCl pH 8), and finally resuspend in 100 ul of Tris buffer. Small aliquots of CO:COLLECTION_SUMMARY unbound and wash fractions were used to analyze the purification quality. CO:SAMPLE_TYPE Mitochondria #TREATMENT TR:TREATMENT_SUMMARY The samples were not subjected to any further treatment. #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Glycerophospholipids: Lipids from isolated mitochondria treated with or without SP:SAMPLEPREP_SUMMARY SMA were extracted using a procedure previously described (Ejsing et al., 2009) SP:SAMPLEPREP_SUMMARY with some modifications: 30-100 µl of sample were brought to a volume of 200 SP:SAMPLEPREP_SUMMARY µl with 155 mM ammonium carbonate buffer. Lipids were extracted by adding 990 SP:SAMPLEPREP_SUMMARY µl of chloroform/methanol 17:1 (v/v) and internal standards (125 pmol PC SP:SAMPLEPREP_SUMMARY 17:0-20:4, 138 pmol PE 17:0-20:4, 118 pmol PI 17:0-20:4, 118 pmol PS 17:0-20:4, SP:SAMPLEPREP_SUMMARY 61 pmol PG 17:0/20:4, 72 pmol PA 17:0/20:4, 10 µl Cardiolipin Mix I; Avanti SP:SAMPLEPREP_SUMMARY Polar Lipids), followed by shaking at 900 rpm/min in a ThermoMixer (Eppendorf) SP:SAMPLEPREP_SUMMARY at 20 °C for 30 min. After centrifugation (12,000xg, 5 min, 4 °C), the lower SP:SAMPLEPREP_SUMMARY (organic) phase was transferred to a new tube, and the upper phase was extracted SP:SAMPLEPREP_SUMMARY again with 990 mL chloroform/methanol 2:1 (v/v). The combined organic phases SP:SAMPLEPREP_SUMMARY were dried under a stream of nitrogen. The residues were resolved in 200 µl of SP:SAMPLEPREP_SUMMARY methanol. Ceramides and sphingomyelins: For the analysis of ceramides and SP:SAMPLEPREP_SUMMARY sphingomyelins in isolated mitochondria without and after SMA treatment, lipids SP:SAMPLEPREP_SUMMARY were extracted as described above in the presence of 127 pmol ceramide 12:0 and SP:SAMPLEPREP_SUMMARY 124 pmol sphingomyelin 12:0 (internal standards, Avanti Polar Lipids). The dried SP:SAMPLEPREP_SUMMARY extracts were resolved in 100 µL of Milli-Q water and 750 µL of SP:SAMPLEPREP_SUMMARY chloroform/methanol 1:2 (v/v). Alkaline hydrolysis of glycerolipids was SP:SAMPLEPREP_SUMMARY conducted as previously published (Schwamb et al., 2012; Oteng et al., 2017). SP:SAMPLEPREP_SUMMARY Fatty acids: To 100 µl of a suspension of isolated mitochondria in PBS, 500 µl SP:SAMPLEPREP_SUMMARY of methanol, 250 µl of chloroform, and 0.5 µg palmitic-d31 acid SP:SAMPLEPREP_SUMMARY (Sigma-Aldrich) as internal standard were added. The mixture was sonicated for 5 SP:SAMPLEPREP_SUMMARY min, and lipids were extracted in a shaking bath at 48 °C for 1 h. SP:SAMPLEPREP_SUMMARY Glycerolipids were degraded by alkaline hydrolysis adding 75 µl of 1 M SP:SAMPLEPREP_SUMMARY potassium hydroxide in methanol. After 5 min of sonication, the extract was SP:SAMPLEPREP_SUMMARY incubated for 1.5 h at 37 °C, and then neutralized with 6 µl of glacial acetic SP:SAMPLEPREP_SUMMARY acid. 2 ml of chloroform and 4 ml of water were added to the extract which was SP:SAMPLEPREP_SUMMARY vortexed vigorously for 30 sec and then centrifuged (4,000 × g, 5 min, 4 °C) SP:SAMPLEPREP_SUMMARY to separate layers. The lower (organic) phase was transferred to a new tube, and SP:SAMPLEPREP_SUMMARY the upper phase extracted with additional 2 ml of chloroform. The combined SP:SAMPLEPREP_SUMMARY organic phases were dried under a stream of nitrogen. The residues were resolved SP:SAMPLEPREP_SUMMARY in 200 µl of acetonitrile/water 2:1 (v/v) and sonicated for 5 min. After SP:SAMPLEPREP_SUMMARY centrifugation (12,000 × g, 20 min, 4 °C), 40 µl of the clear supernatants SP:SAMPLEPREP_SUMMARY were transferred to autoinjector vials. References: Ejsing et al., Proc Natl SP:SAMPLEPREP_SUMMARY Acad Sci USA 2009, 106, 2136; Oteng et al., J Lipid Res 2017, 58, 1100; Schwamb SP:SAMPLEPREP_SUMMARY et al., Blood 2012, 120, 3978. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_SUMMARY Note: Macherey-Nagel does not offer this column as standard, but manufactures it CH:CHROMATOGRAPHY_SUMMARY on request. CH:CHROMATOGRAPHY_TYPE Normal phase CH:INSTRUMENT_NAME Agilent 1260 CH:COLUMN_NAME Macherey-Nagel Nucleosil NH2 (50×2 mm, 3 µm, 120 Å) CH:SOLVENT_A 97% acetonitrile/2% methanol/1% acetic acid; 5 mM ammonium acetate CH:SOLVENT_B 99% methanol/1% acetic acid; 5 mM ammonium acetate CH:FLOW_GRADIENT 0 min: 0% B, 0.5 min: 0% B, 0.7 min: 10% B, 1.2 min: 10% B, 1.6 min: 18% B, 2.2 CH:FLOW_GRADIENT min: 18% B, 2.6 min: 100% B, 4.5 min: 100% B, 4.9 min: 0% B, 6.5 min: 0% B CH:FLOW_RATE 0.75 ml/min CH:COLUMN_TEMPERATURE 20 #ANALYSIS AN:ANALYSIS_TYPE MS #MS MS:INSTRUMENT_NAME SCIEX QTRAP 6500 MS:INSTRUMENT_TYPE QTRAP MS:MS_TYPE ESI MS:ION_MODE POSITIVE MS:MS_COMMENTS LC-ESI-MS/MS analysis of ceramides and sphingomyelins was conducted as MS:MS_COMMENTS previously published (Oteng et al., J Lipid Res 2017, 58, 1100; Schwamb et al., MS:MS_COMMENTS Blood 2012, 120, 3978). #MS_METABOLITE_DATA MS_METABOLITE_DATA:UNITS counts per second (cps) MS_METABOLITE_DATA_START Samples S01_mitos_control.SMA_1 S02_mitos_control.SMA_2 S03_mitos_control.SMA_3 S04_mitos_control.SMA_4 S05_mitos_apoptosis.SMA_1 S06_mitos_apoptosis.SMA_2 S07_mitos_apoptosis.SMA_3 S08_mitos_apoptosis.SMA_4 S09_mitos_control_1 S10_mitos_control_2 S11_mitos_control_3 S12_mitos_control_4 S13_mitos_apoptosis_1 S14_mitos_apoptosis_2 S15_mitos_apoptosis_3 S16_mitos_apoptosis_4 S02_pulldown_Control_22.08 S03_pulldown_Control_01.09 S04_pulldown_Control_04.09 S05_pulldown_Control_31.09 S06_pulldown_Apoptosis_22.08 S07_pulldown_Apoptosis_01.09 S08_pulldown_Apoptosis_04.09 S09_pulldown_Apoptosis_31.09 Factors Sample source:mitochondrial SMALPs | Genotype:WT | Condition:control Sample source:mitochondrial SMALPs | Genotype:WT | Condition:control Sample source:mitochondrial SMALPs | Genotype:WT | Condition:control Sample source:mitochondrial SMALPs | Genotype:WT | Condition:control Sample source:mitochondrial SMALPs | Genotype:WT | Condition:apoptotic Sample source:mitochondrial SMALPs | Genotype:WT | Condition:apoptotic Sample source:mitochondrial SMALPs | Genotype:WT | Condition:apoptotic Sample source:mitochondrial SMALPs | Genotype:WT | Condition:apoptotic Sample source:total mitochondria | Genotype:WT | Condition:control Sample source:total mitochondria | Genotype:WT | Condition:control Sample source:total mitochondria | Genotype:WT | Condition:control Sample source:total mitochondria | Genotype:WT | Condition:control Sample source:total mitochondria | Genotype:WT | Condition:apoptotic Sample source:total mitochondria | Genotype:WT | Condition:apoptotic Sample source:total mitochondria | Genotype:WT | Condition:apoptotic Sample source:total mitochondria | Genotype:WT | Condition:apoptotic Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:control Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:control Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:control Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:control Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:apoptotic Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:apoptotic Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:apoptotic Sample source:mitochondrial SMALPs | Genotype:mEGFP-BAK | Condition:apoptotic Cer 18:1;O2/12:0 (IS) 62854554 66209758 76873410 62776237 66938341 70040240 69846020 55922546 60251711 42608445 64366517 76913545 68460397 65026514 56585330 53587576 107295534 76440194 55636065 20219126 53473727 35729833 28589720 45754100 Cer 18:1;O2/14:0 166415 208355 189673 85612 241639 238379 187905 262696 108619 42847 833284 189174 625663 833130 575225 922375 54628 60939 70284 20596 80650 40781 57245 58972 Cer 18:1;O2/16:0 707079 525720 690265 475657 943034 556643 736912 859080 1514192 287945 5020098 2323094 3599368 2254612 4836885 8097698 247019 195254 260178 117059 132863 124388 106748 96899 Cer 18:1;O2/16:1 289452 332987 438022 265762 317874 320797 328156 360552 275592 130881 622463 426974 700192 601219 595320 813611 217817 139110 145039 86629 137624 77460 78342 103079 Cer 18:1;O2/18:0 93010 107007 119940 82956 107019 101993 100859 102582 146936 50274 344456 216836 262172 177972 176149 169199 75767 53411 46076 37775 36005 27653 27684 27707 Cer 18:1;O2/18:1 29327 29014 47621 24465 36606 33880 46105 86331 42774 27466 274240 99960 242440 239012 267747 427941 51996 11806 101465 11690 24882 39461 41404 22650 Cer 18:1;O2/20:0 22718 24718 46116 21250 31901 29923 46415 44691 30617 17747 162891 59629 67937 113359 171829 259566 35982 25331 83529 17608 37049 49150 70862 24721 Cer 18:1;O2/22:0 53712 61803 63359 45166 80599 68236 73786 82794 103043 19376 279595 160076 195535 129368 208687 241106 30483 29338 24664 16673 17727 13579 12779 12359 Cer 18:1;O2/22:1 11014 9410 11667 8575 16362 13486 12635 15043 15588 5762 41525 24694 38205 18043 20130 19403 7500 5179 5371 4541 3759 3121 3853 2391 Cer 18:1;O2/24:0 187281 226426 296324 200302 313191 230086 297621 308867 419198 42552 1148856 656941 504490 318797 452145 227250 94265 76360 64128 32368 64401 64696 43775 29789 Cer 18:1;O2/24:1 279410 258716 323549 225698 450891 308540 360553 396209 588662 112780 1692830 945729 806230 421998 514107 332136 81002 72089 68419 26702 56178 58041 54028 31800 Cer 18:1;O2/26:0 24565 44345 45400 24399 33665 37397 37108 32777 28729 22835 86587 50959 105102 31845 42370 32021 24906 22067 15368 15627 14382 8135 12982 29284 Cer 18:1;O2/26:1 38241 34264 41480 29396 59842 35117 42629 43848 63750 11172 182126 99098 133229 49789 63645 47075 20883 13299 13715 7619 13277 11260 10399 7766 SM 18:1;O2/12:0 (IS) 12278792 8012135 9560593 7234260 10909370 9227934 8042176 8749546 5192979 4388543 7294405 4783978 3249252 5459398 3762596 4763562 6031436 2810836 3941971 1920769 2293461 2767661 1995166 2167435 SM 18:1;O2/14:0 94606 88883 97895 75260 96677 109968 97544 123902 521547 218511 1491490 442204 276249 391301 275626 294585 21415 6285 18044 6028 9765 7941 7990 7464 SM 18:1;O2/16:0 1044344 1008021 1212627 834530 1063265 1237416 1053088 1250897 6031564 2560988 16194169 5372633 3290884 4498409 3336856 3452847 389702 152442 245607 126936 147996 153156 161516 154746 SM 18:1;O2/16:1 135962 142415 186793 119620 149586 186110 170172 191336 763525 303735 2398036 691627 432825 552671 402177 407760 27405 7243 18256 8005 15089 8657 13470 7519 SM 18:1;O2/18:0 98812 71843 82240 62439 83545 87095 74666 88364 193565 96396 496849 171180 113825 175555 125032 136740 62013 26380 39298 18462 19894 22488 20273 19994 SM 18:1;O2/18:1 19778 21898 20443 17934 19555 23781 16943 25092 87686 35811 258691 75775 50481 69176 50008 48866 10872 6004 6245 2119 2866 2010 3230 1758 SM 18:1;O2/20:0 11950 11006 13824 14339 11565 14205 20162 20171 57791 23703 188498 45994 31681 45782 46420 35841 9121 7809 8264 7643 4029 3150 3742 3765 SM 18:1;O2/22:0 19645 16031 24899 26856 22605 23994 27927 27339 108638 40384 288152 81887 50841 116251 82936 72392 16353 17437 10521 11950 5891 6095 6293 7965 SM 18:1;O2/22:1 17822 19579 21952 18626 19923 25394 23006 26170 88713 34253 247953 76712 45124 73197 52106 47383 5597 2363 3951 1843 2727 1679 2817 1881 SM 18:1;O2/24:0 25741 31007 47903 45112 33838 51633 46302 46632 261345 92297 667979 208439 120022 223134 180211 162189 15274 7398 11608 4912 9390 5353 6031 5704 SM 18:1;O2/24:1 126286 137234 178388 128190 135651 201226 161674 187597 790747 312198 2093246 688227 432088 604605 436120 430516 33083 13053 25564 8287 18209 9612 14881 9439 SM 18:1;O2/26:0 2641 1953 3475 3172 3212 3322 3803 3636 11973 4405 31766 8872 5933 11287 9460 7454 753 248 1117 577 635 657 361 490 SM 18:1;O2/26:1 5464 4928 7479 5617 6445 7777 7781 8506 30601 11073 75934 24921 17729 28354 18498 17424 2471 1205 1717 629 1594 871 998 783 MS_METABOLITE_DATA_END #METABOLITES METABOLITES_START metabolite_name Q1 Mass (Da) Q3 Mass (Da) RT (min) CE (volts) PubChem_CID LM_ID Cer 18:1;O2/12:0 (IS) 482.6 264.4 0.32 35 5283562 LMSP02010002 Cer 18:1;O2/14:0 510.6 264.4 0.32 36 5282310 LMSP02010001 Cer 18:1;O2/16:0 538.7 264.4 0.32 37 5283564 LMSP02040003 Cer 18:1;O2/16:1 536.7 264.4 0.32 37 N/A N/A Cer 18:1;O2/18:0 566.7 264.4 0.32 39 5283565 LMSP02010006 Cer 18:1;O2/18:1 564.7 264.4 0.32 39 5283563 LMSP02010003 Cer 18:1;O2/20:0 594.7 264.4 0.32 41 5283566 LMSP02010007 Cer 18:1;O2/22:0 622.8 264.4 0.32 41 5283567 LMSP02010008 Cer 18:1;O2/22:1 620.8 264.4 0.32 41 N/A N/A Cer 18:1;O2/24:0 650.9 264.4 0.32 43 5283571 LMSP02010012 Cer 18:1;O2/24:1 648.9 264.4 0.32 43 5283568 LMSP02010009 Cer 18:1;O2/26:0 678.9 264.4 0.32 45 5283570 LMSP02010011 Cer 18:1;O2/26:1 676.9 264.4 0.32 45 5283569 LMSP02010010 SM 18:1;O2/12:0 (IS) 647.7 184.4 4.17 39 44260123 LMSP03010002 SM 18:1;O2/14:0 675.7 184.4 4.16 40 11433862 LMSP03010028 SM 18:1;O2/16:0 703.8 184.4 4.15 41 9939941 LMSP03010003 SM 18:1;O2/16:1 701.8 184.4 4.15 41 52931145 LMSP03010041 SM 18:1;O2/18:0 731.8 184.4 4.13 43 6453725 LMSP03010001 SM 18:1;O2/18:1 729.8 184.4 4.13 43 6443882 LMSP03010029 SM 18:1;O2/20:0 759.8 184.4 4.13 44 44260124 LMSP03010005 SM 18:1;O2/22:0 787.9 184.4 4.12 44 44260125 LMSP03010006 SM 18:1;O2/22:1 785.9 184.4 4.12 44 52931203 LMSP03010072 SM 18:1;O2/24:0 815.9 184.4 4.11 45 44260127 LMSP03010008 SM 18:1;O2/24:1 813.9 184.4 4.11 45 44260126 LMSP03010007 SM 18:1;O2/26:0 843.9 184.4 4.09 47 44260129 LMSP03010010 SM 18:1;O2/26:1 841.9 184.4 4.09 47 44260128 LMSP03010009 METABOLITES_END #END