Technical Abstract: Aflatoxins are potent carcinogens that are produced by certain Aspergillus fungi. The aflatoxins were first discovered in the 1960s and since that time have been found to be distributed worldwide in a variety of commodities, foods, and feeds. Many of the early techniques for detecting aflatoxins involved extraction with halogenated solvents. With the increased availability and use of reverse-phase solid phase extraction cartridges and the availability of immunoaffinity columns, aqueous mixtures of non-halogenated solvents have been frequently used. To further reduce the need for solvents we examined the effects of eliminating solvents during the extraction of maize using aqueous mixtures of the detergent sodium dodecyl sulfate (SDS). Following extraction and filtration, aflatoxins B1 and G1 (AFB1, AFG1) were isolated using commercially available immunoaffinity columns. The isolated AFB1 and AFG1 were derivatized with trifluoroacetic acid before separation by liquid chromatography and detection by fluorescence. In spiked maize the limits of detection were 0.5 ng/g and 1 ng/g for AFB1 and AFG1 respectively. Recoveries of AFB1 spiked into maize between 1 and 20 ng/g, averaged 87.5% (range 76.3% to 99.0%), with an average repeatability standard deviation (RSDr) of 4.0%. Recoveries of AFG1 spiked into maize between 2 and 20 ng/g averaged 80.4% (range 70.3% to 85.8%), with an average RSDr of 3.5%. This is the first reported demonstration of an effective solvent-free extraction of aflatoxins from maize at ambient pressure, and may serve to help reduce solvent consumption during aflatoxin analysis.