Simultaneous analysis of pyrethrins (Py-I and Py-II) and piperonyl butoxide (PBO) in soil and runoff water samples following field application of a new pyrethrum formulation containing pyrethrins (Py's) and PBO is described. Residues of total Py's and PBO were extracted from soil samples using hexane-acetone (9:1). A solid phase extraction (SPE) column containing C18-octadecyl bonded silica was used to separate Py's and PBO residues from runoff water. Residues in soil and water were quantitated by high performance liquid chromatography (HPLC) equipped with C18-column and a UV detector. Concentration of Py-II in soil was 100 times higher than that of Py-I 1 h following treatment and 9.6 times higher than Py-I in runoff surface water 11 days following treatment. Results indicated that Py's are non-persistent in soil (even though lipophillic) and water when applied at the recommended rate of 6 lbs (5.31 g A.I.) per acre. There was a consistent decrease in total Py's residues as time after spraying increased. Py's residues in soil decreased from 0.91 to 0.11 ppm 4 days following treatment and one month after treatment only 0.002 ppm were detected. The highest concentration of Py's in runoff water was 36.09 ng/liter following the first rainfall (11 days following treatment). PBO initial residues detected in soil samples were low (0.84 microgram/g soil) while no residues of PBO were detected in runoff water.