A multiresidue procedure was developed for analysis of cotton pesticide and harvest-aid chemicals in water using solid-phase extraction and analysis by GC-NPD, GC-MS, and HPLC-DAD. Target compounds included the defoliants tribufos, dimethipin, thidiazuron; the herbicide diuron; and the insecticide methyl parathion. Three solid-phase extraction (SPE) media, octadecylsilyl (ODS), graphitized carbon black (GCB), and a divinylbenzene-N-vinyl pyrollidine copolymer (DVBVP), were evaluated. On GCB and ODS, recoveries varied depending on compound type. Recoveries were quantitative for all compounds on DVBVP, ranging from 87 to 115% in spiked deionized water and surface runoff. The method detection limit was less than 0.1 microg L(-)(1). SPE with DVBVP was applied to post-defoliation samples of surface runoff and tile drainage from a cotton research plot and surface runoff from a commercial field. The research plot was defoliated with a tank mixture of dimethipin and thidiazuron, and the commercial field, with tribufos. Dimethipin was detected (1.9-9.6 microg L(-)(1)) in all research plot samples. In the commercial field samples, tribufos concentration ranged from 0.1 to 135 microg L(-)(1). An exponentially decreasing concentration trend was observed with each successive storm event.