Magnetic framework composite (Fe3O4@TMU-12) microspheres were successfully synthesized and applied as an effective sorbent for preconcentration of diazinon in environmental water samples. Magnetic framework composite nanospheres were fabricated by a step-by-step assembly strategy. The extraction conditions and efficiency of the magnetic framework composite nanospheres for diazinon were investigated. The method was evaluated according to the reproducibility, preconcentration factor, linearity range and limits of detection. Under optimal conditions, the preconcentration factors and relative recoveries of the studied compound was obtained in the range of 210 and 90.5–99.0%, respectively. The calibration curve was obtained in the range of 5–200 μg/L with reasonable linearity (R2 >0.99) and the limits of detection (LODs) 2 μg/L (based on S/N = 3). The relative standard deviations of intra- and inter-day tests 5.2 and 6.3%, respectively. Determination of diazinon can be easily carried out with this fast, accurate, sensitive and simple method procedure.