As part of a collaborative study involving the United States Geological Survey Toxics Substances Hydrology Project (Toxics Project) and the University of California, Davis, Bodega Marine Laboratory (BML), water samples were collected at three sites within the San Joaquin River Basin of California and analyzed for dissolved pesticides. Samples were collected during, and immediately after, the first significant rainfall (greater than 0.5 inch per day) following the local application of dormant spray, organophosphate insecticides during the winters of 2000 and 2001. All samples were collected in conjunction with fish-caging experiments conducted by BML researchers. Sites included two locations potentially affected by runoff of agricultural chemicals (San Joaquin River near Vernalis, California, and Orestimba Creek at River Road near Crows Landing, California), and one control site located upstream of pesticide input (Orestimba Creek at Orestimba Creek Road near Newman, California). During these experiments, fish were placed in cages and exposed to storm runoff for up to ten days. Following exposure, the fish were examined for acetylcholinesterase concentrations and overall genetic damage. Water samples were collected throughout the rising limb of the stream hydrograph at each site for later pesticide analysis. Concentrations of selected pesticides were measured in filtered water samples using solid-phase extraction (SPE) and gas chromatography-mass spectrometry (GC/MS) at the U.S. Geological Survey organic chemistry laboratory in Sacramento, California. Results of these analyses are presented.