Dust collected in New Orleans homes mold-contaminated because of the flooding after hurricane Katrina was analyzed for molds and mycotoxins. The mycoflora was studied by cultivation and quantitative PCR for selected molds. The most commonly found mold taxa were Aspergillus, Cladosporium, and Penicillium. Verrucarol, a hydrolysis product of macrocyclic trichothecenes predominately produced by Stachybotrys spp. was identified in three dust samples by gas chromatography-tandem mass spectrometry, and sterigmatocystin (produced by various Aspergillus spp.) was found in two samples by high pressure liquid chromatography-tandem mass spectrometry. This is the first demonstration of mycotoxins in Katrina-associated dust samples. The analytical methods used represent valuable tools in further studies on bioaerosol exposure and health risks.