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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), Column: TSKgel-100V (4.6 x 250 mm, 5 micrometer; TOSOH), Solvent: A; 0.1% formic acid aq. B; ACN (addition 0.1% formic acid fc.), Gradient: (B);3 to 97% (0.0 to 45.0 min), 97% (45.0 to 50.0 min), 97% to 3% (50 to 50.1 min), 3% (50.1 to 57.0 min), Column temp.: 40 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=100000 o(100.0-1500.0); 2: ITMS + c norm !corona !pi Dep MS/MS Most intense ion from (1); 3: ITMS + c norm !corona !pi Dep MS/MS 2nd most intense ion from (1); 4: ITMS + c norm !corona !pi Dep MS/MS 3rd most intense ion from (1); 5: ITMS + c norm !corona !pi Dep MS/MS 4th most intense ion from (1); 6: ITMS + c norm !corona !pi Dep MS/MS 5th most intense ion from (1)., Rejected mass=224.0100, 235.1800, 241.0700, 266.2300, 282.1000, 315.0900, 376.0400, 378.0400, 389.1100, 463.1300, 480.1600, 534.0500, 537.1500, 540.6000, 554.1800, 609.2800, 628.2000, 702.2200, 726.3600, 810.4200, 1101.7000, 1118.7200, 1123.6800 810.4200, 1101.7000, 1118.7200, 1123.6800
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