Application of Tagetes minuta floral extract to silica gel column chromatography produced 2 fractions with the hydrogenate part 20-30 times more toxic to larvae and 12-13 times more toxic to adults of Aedes aegypti and Anopheles stephensi, respectively, than the oxygenate part. Further fractionation by column chromatography of the hydrogenate fraction produced 4 thiophenes, 5-(but-3-ene-1-ynyl)-2,2'-bithiophene, 5-(but-3-ene-1-ynyl)-5'-methyl-2,2'-bithiophene, 2,2',5',2"-terthiophene, and 5-methyl-2,2',5',2"-terthiophene. These compounds in Tagetes minuta are largely responsible for the toxicity exhibited against the tested mosquitoes.