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The LC-MS/MS was performed on both polar and hydrophobic metabolites using an Ultimate 3000 RSLC nano coupled to an HPG pump or a Vanquish Flex UPLCs coupled to Orbitrap Fusion Lumos Tribrid mass spectrometer (Thermo Fisher Scientific) in HILIC LC-MS and RP-LC-MS, operated in positive and negative ionization modes as described previously 30