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A 10 L aliquot of the filtered extract was injected on to a Zorbax RX-SIL column (2.1 mm 150 mm, 5 m) (Agilent Technologies) pre-equilibrated with a mixture of 10% solvent A (15 mM ammonium formate) and 90% solvent B (acetonitrile) connected to an Agilent 1260 Infinity HPLC