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The fractions were separated by nano-high-performance LC (Eksigent Technologies, Dublin, CA, United States) on a secondary RP analytical column (Eksigent, C18, 3 m, 150 mm 75 m) using a gradient mobile phase of 98% acetonitrile, 2% Milli-Q water (A) and 0.1% formic acid (B) at a flow rate of 0.3 L/min