A method is described for the analysis of the insecticide imidacloprid [1-(6-chloro-3-pyridylmethyl)-N-nitroimidazolidin-2-ylideneamine] and its metabolite 6-chloronicotinic acid by micellar electrokinetic chromatography with diode-array detection at 270 and 227 nm, respectively. The best results were obtained using sodium dodecyl sulphate at a concentration of 60 mM and a running buffer of NH4Cl/NH3 at 15 mM (pH 8.5). The selection of instrumental parameters such as voltage at 30 kV with an injection time of 20 s gave the best resolution with an analysis time of less than 6 min. The method yields similar sensitivity for the parent compound and for the metabolite, with detection limits of 0.71 and 1.18 microg/ml for imidacloprid and 6-chloronicotinic acid, respectively. The sampling and analysis of these two pesticides in greenhouse air was carried out using personal samplers connected to XAD-2 cartridges as sampling media, investigating the dissipation of analytes in a 24-h period after their application.