#METABOLOMICS WORKBENCH laura_capolupo_20210210_062234 DATATRACK_ID:2468 STUDY_ID:ST001691 ANALYSIS_ID:AN002761 PROJECT_ID:PR001087 VERSION 1 CREATED_ON February 11, 2021, 2:13 pm #PROJECT PR:PROJECT_TITLE Untargeted lipidomics of primary human skin fibroblasts PR:PROJECT_TYPE MS qualitative untargeted lipidomics of human fibroblasts PR:PROJECT_SUMMARY Untargeted lipidomics of primary human skin fibroblasts to identify their PR:PROJECT_SUMMARY lipidome in positive ion mode PR:INSTITUTE École polytechnique fédérale de Lausanne (EPFL) PR:LABORATORY UPDANGELO PR:LAST_NAME Capolupo PR:FIRST_NAME Laura PR:ADDRESS Route Cantonale, Lausanne, Vaud, 1015, Switzerland PR:EMAIL laura.capolupo@epfl.ch PR:PHONE +41 21 693 42 79 #STUDY ST:STUDY_TITLE LC-MS untargeted lipidomics of primary human fibroblasts ST:STUDY_TYPE LC-MS untargeted lipidomics of fibroblasts ST:STUDY_SUMMARY We did LC-MS untargeted lipidomics of primary human fibroblasts to have a ST:STUDY_SUMMARY comprehensive overview of their lipidome in positive ion mode ST:INSTITUTE École polytechnique fédérale de Lausanne (EPFL) ST:LAST_NAME Capolupo ST:FIRST_NAME Laura ST:ADDRESS Route Cantonale ST:EMAIL laura.capolupo@epfl.ch ST:PHONE +41 21 693 42 79 #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 - 01_01FibroblastSphin1_n1p_A_1 Treatment:methylamine treatment RAW_FILE_NAME=01_01FibroblastSphin1_n1p_A_1; extraction type=MTBE SUBJECT_SAMPLE_FACTORS - 02_02FibroblastSphin2_n1p_A_1 Treatment:methylamine treatment RAW_FILE_NAME=02_02FibroblastSphin2_n1p_A_1; extraction type=MTBE SUBJECT_SAMPLE_FACTORS - 03_03FibroblastTotal1_n1p_A_1 Treatment:total lipid extract RAW_FILE_NAME=03_03FibroblastTotal1_n1p_A_1; extraction type=MTBE SUBJECT_SAMPLE_FACTORS - 04_04FibroblastTotal2_n1p_A_1 Treatment:total lipid extract RAW_FILE_NAME=04_04FibroblastTotal2_n1p_A_1; extraction type=MTBE #COLLECTION CO:COLLECTION_SUMMARY Cells were washed with cold PBS, scraped and collected after centrifugation in CO:COLLECTION_SUMMARY -80° untill the MS analysis CO:SAMPLE_TYPE Fibroblasts #TREATMENT TR:TREATMENT_SUMMARY No treatment has been done on the cells #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Total lipid extracts were prepared using a standard MTBE protocol followed by a SP:SAMPLEPREP_SUMMARY methylamine treatment for total lipid analysis by mass spectrometry 7. Briefly, SP:SAMPLEPREP_SUMMARY cell pellet was resuspended in 100 μL H2O. 360 μL methanol and 1.2 mL of MTBE SP:SAMPLEPREP_SUMMARY were added and samples were placed for 10 min on a vortex at 4 °C followed by SP:SAMPLEPREP_SUMMARY incubation for 1 h at room temperature on a shaker. Phase separation was induced SP:SAMPLEPREP_SUMMARY by addition of 200 μL of H2O. After 10 min at room temperature, samples were SP:SAMPLEPREP_SUMMARY centrifuged at 1000 g for 10 min. The upper (organic) phase was transferred into SP:SAMPLEPREP_SUMMARY a glass tube and the lower phase was re-extracted with 400 μL artificial upper SP:SAMPLEPREP_SUMMARY phase [MTBE/methanol/H2O (10:3:1.5, v/v/v)]. The combined organic phases were SP:SAMPLEPREP_SUMMARY dried in a vacuum concentrator. Lipids where then resuspended in 500 μL of SP:SAMPLEPREP_SUMMARY CHCl3 and divided in two aliquots for a further methylamine treatment for SP:SAMPLEPREP_SUMMARY sphingo- and glycosphingolipids analysis. In details, 500 μL of freshly SP:SAMPLEPREP_SUMMARY prepared monomethylamine reagent [methylamine/H2O/nbutanol/ methanol (5:3:1:4, SP:SAMPLEPREP_SUMMARY (v/v/v/v)] was added to the dried lipid extract and then incubated at 53 °C for SP:SAMPLEPREP_SUMMARY 1 h in a water bath. Lipids were cooled to room temperature and then dried. The SP:SAMPLEPREP_SUMMARY dried lipid extract was then extracted by n-butanol extraction using 300 μL SP:SAMPLEPREP_SUMMARY water-saturated nbutanol and 150 μL H2O. The organic phase was collected, and SP:SAMPLEPREP_SUMMARY the aqueous phase was reextracted twice with 300 μL water-saturated n-butanol. SP:SAMPLEPREP_SUMMARY The organic phases were pooled and dried in a vacuum concentrator. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_SUMMARY Liquid chromatography on a HILIC Column CH:CHROMATOGRAPHY_TYPE HILIC CH:INSTRUMENT_NAME Shimadzu Prominence UFPLC xr system CH:COLUMN_NAME Kinetex ( 2.6lm, 2.1 × 50 mm2) CH:METHODS_FILENAME laura_capolupo_20210210_062234_PR_CH_Chromatography_methods.pdf #ANALYSIS AN:ANALYSIS_TYPE MS AN:ANALYSIS_PROTOCOL_FILE laura_capolupo_20210210_062234_PR_MS_MS_methods.pdf #MS MS:INSTRUMENT_NAME Hybrid Orbitrap Elite MS:INSTRUMENT_TYPE Orbitrap MS:MS_TYPE ESI MS:ION_MODE POSITIVE MS:MS_COMMENTS Check protocol file MS:MS_RESULTS_FILE ST001691_AN002761_Results.txt UNITS:abundance Has m/z:Yes Has RT:Yes RT units:Minutes #END