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Fraction 4 was subjected to preparative reversed phase HPLC over a Luna PFP(2) (pentafluorophenyl) column (Phenomenex, 250 mm × 21.2 mm, 5 µm) using a gradient of 70:30 to 100:0 CH 3 OH–H 2 O (10 mM of ammonium acetate in both phases) over 20 min at a flow rate of 20 mL/min