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The supernatant was then freeze-dried in a vacuum concentrator (Labconco, CentriVap Benchtop Centrifugal Vacuum Concentrator) at 4 C, then dissolved in 50 L of 50% (v/v, in water) acetonitrile with formic acid, and vortexed three times for 30 s, followed by centrifugation at 14,000 g for another 10 min at 4 C

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