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The extract was rotary evaporated at 30 C to a volume of 2 ml, acidified to pH 4 with formic acid, and 200 l aliquots were purified using preparative HPLC (Agilent Technologies, 1260 Infinity) over a Luna 5 m phenyl-hexyl 100 (250 10 mm) column and a 15 min linear gradient from 0% acetonitrile in H 2 O to 16% acetonitrile in H 2 O at 4 ml min 1 flow