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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 μl aliquots were purified using preparative HPLC (Agilent Technologies, 1260 Infinity) over a Luna 5 µm phenyl-hexyl 100 Å (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
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