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Samples were eluted with isocratic flow 2/98 (acetonitrile/ammonium formate, pH 2.5) for 2 min, followed by gradient from 2/98 to 70/30 in 1 min, then isocratic mobile phase 70/30 (acetonitrile/ammonium formate, pH 2.5) for 2 min, and a final gradient from 70/30 to 2/98 (acetonitrile/ammonium formate, pH 2.5) for 3 min

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