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Harvested sample is frozen by liquid N2 an … Harvested sample is frozen by liquid N2 and resulting powder (100mg) are solved in 300uL 80% methanol solution. 20uL sample is injected into HPLC after 0.2um membrane filter treatment. HPLC conditions: Agilent 1100 series (Agilent), Solvent: A; 0.1% formic acid aq. B; ACN (addition 0.1% formic acid fc.), Gradient: (B);3 to 40% (0.0 to 23.0 min), 40 to 95% (23.0 to 23.1 min), 95% (23.1 to 25.0 min), 3% (25.1 to 30.0 min), Column temp.: 30 degree C, Flow rate=0.5mL/min, PDA: 200-650 nm (2 nm step). FT-ICR-MS conditions: Filter 1: FTMS + c norm !corona !pi res=50000 o(200.0-1500.0), Rejected mass=266.0000;294.0000;391.0000. Rejected mass=266.0000;294.0000;391.0000.
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