Abstract. A new method has been developed for the analysis of fumonisin B, in corn using capillary electrophoresis. Fumonisin B, is the major fumonisin metabolite produced by the fungus Fusarium moniliforme and has been implicated in human and animal diseases. Fumonisin B, was extracted from corn with acetonitrile/water (SO/SO) and cleaned up with a Waters C,, Sep-Pak Vac cartridge. Fumonisin B, was quantitated after elution from the C,, Sep-Pak column using capillary electrophoresis (CE) with a 25 mM sodium borate buffer (pH 9.0) containing 10% acetonitrile and fluorescence detection of the FMOC derivative. The minimum detectable amount in corn was 0.5 ppm. Recovery values in spiked corn averaged over 96% over the range 1-20 ppm. o 1995 John Wiley & Sons, Inc.