A rapid, easy to operate, and sensitive method was developed for the trace determination of benzoylurea insecticides based on a micro-solid phase extraction with highly ordered TiO2 nanotube arrays as the adsorbent prior to high performance liquid chromatography. The experimental results indicated that a good linear relationship was achieved between the peak areas and the concentrations of benzoylurea insecticides in the range of 0.1–40 μg L−1. The limits of detection (LODs) of diflubenzuron, chlorbenzuron, triflumuron and chlorfluazuron were 0.082, 0.026, 0.049 and 0.076 μg L−1, respectively. The proposed method was successfully used to determine the benzoylurea insecticides in environmental water samples. The spiked recoveries in the range of 76.5–102.4% were achieved. All these results demonstrated that the proposed method was of great value and would have great potential in the enrichment and determination of trace pollutants in the future.
