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Phenomenex, Aschaffenburg, Germany) to remove remaining cell debris, made up to 10 mL with MeOH and, then, analyzed by means of UPLC-TOF MS using the following chromatographic conditions (0.4 mL/min, 40 C): starting with a mixture of H 2 O/MeOH (10/90, v/v), the MeOH content was kept constant for 1 min at 90%, increased to 100% within 8 min, kept constant for 1 min, decreased within 0.1 min to 90% MeOH, followed by re-equilibration for 0.4 min