A microextraction technique of solid phase membrane tip extraction (SPMTE) prior to gas chromatograph was developed to determine fifteen pesticides (organochlorine (OCPs) and pyrethroid). In the SPMTE procedure, multiwalled carbon nanotubes (MWCNTs) were used as the adsorbent enclosed in SPMTE device and then several important parameters influenced extraction efficiency were comprehensively optimized. Under the optimum conditions, the method obtaine good linearity in the range of 1–500.0 and 1.5–750.0 ng mL-1for OCPs and pyrethroid pesticides, low limits of detection in the range of 0.018–1.064 ng mL-1(S/N=3). Seven target analytes are detected in river sample, none of the other samples tested show any pesticide residue. The developed method is a simple, feasible, and inexpensive microextraction technique.