High performance liquid chromatography (HPLC) separation coupled to a tandem quadrupole mass spectrometer (MS) via an atmospheric pressure electrospray ionisation interface provides an extremely powerful tool for rapid, selective and sensitive analysis of plant protection products in crops. A residue analytical method was developed using this technique for the quantitative determination of the insecticide triazamate and all of its major metabolites in sugar beet and apple in one single chromatographic run. The limit of quantification (LOQ) proved to be at 0.01 or 0.02 mg/kg.