Abstract--The basin of the Corumbataí despite their considerable state of preservation, as regards quantity and quality of water, deserves special attention since provide 100% of supply in the city of Piracicaba, SP and other municipalities. Furthermore, in these cities it's expressive the intensive use of land for sugar cane cultivation, where it is used, among other inputs, the pesticide fipronil. Despite the great importance of the basin for the region, there are few studies that demonstrate the impact of agriculture and intensive use of pesticides in water quality. Thus this study has as objective of the environmental monitoring in the basin of the Corumbataí, determining the occurrence of residues of the pesticides fipronil and a group of organochlorines (OCPs), which are: alachlor, chlordane, endosulfan, heptachlor and heptachlor epoxide, lindane, metolachlor and methoxychlor in waters from differents collection points, and validate the methodology for extraction and analysis by gas chromatography (GC-MS). The samples analyzed (40) presented levels of OCPs and fipronil lower than allowed by Brazilian legislation.