Rapid purification of fumonisins and their hydrolysis products with solid-phase extraction columns |
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| Authors: | Poling S M Plattner R D |
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| Institution: | Mycotoxin Research, National Center for Agricultural Utilization Research, Agricultural Research Service, U.S. Department of Agriculture, Peoria, IL 61604, USA. polingsm@mail.ncaur.usda.gov |
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| Abstract: | Fumonisins B(3) and B(4) (FB(3) and FB(4)) were recovered from the 50:50 acetonitrile/water extract of corn cultures of a strain of Fusarium moniliforme that does not make FB(1) or FB(2) by stirring the extract with IRA-68, a weak anion-exchange resin. The fumonisins were desorbed with 5% acetic acid in the same solvent. After dilution with water, the desorbed fumonisins were separated into FB(3) (FB(3) and FA(3)) and FB(4) (FB(4), FC(4), and FA(4)) fractions with a tC(18) solid-phase extraction (SPE) cartridge. The FB(3) fraction was then separated into FB(3) and FA(3) by using an NH(2) SPE cartridge and eluting with 5% acetic acid and increasing amounts of acetonitrile in water. Finally, FB(1) and FA(3) were hydrolyzed with calcium hydroxide. After recovery from the reaction mixture using a tC(18) cartridge, the hydrolyzed and partially hydrolyzed analogues were separated and the unreacted fumonisins recovered by using an NH(2) cartridge, initially in the normal-phase mode with increasing amounts of water in acetonitrile and then in the reversed-phase mode after the addition of 5% acetic acid to the solvent and eluting in the reverse order. |
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