▎ 摘　　要

NOVELTY - Preparing three-dimensional graphene material modified by zirconium dioxide nanoparticles involves: (a) corroding metal mesh with dilute hydrochloric acid, and drying; (b) placing the metal mesh with rough surface after corrosion in 3-aminopropyltriethoxysilane to realize amination of metal mesh; (c) adding polydiallyldimethylammonium chloride to a graphene oxide suspension, and then adding aminated metal mesh, N,N-hydroxysuccinimide and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide as a catalyst for reaction; (d) repeating operations (b) and (c) three times in sequence on the metal mesh obtained in step (c) to obtain a graphene oxide-modified metal mesh; and (e) placing graphene oxide-modified metal mesh in zirconyl chloride octahydrate solution, adding ammonia, reacting, and freeze drying in a freeze dryer. USE - The method is useful for preparing three-dimensional graphene material modified by zirconium dioxide nanoparticles used as filler in solid phase extraction column used for detection of organophosphorus pesticide (all claimed) in vegetables. ADVANTAGE - The method provides nanoparticles, which detect organophosphorus pesticide with wide linear range, low detection limit, high sensitivity and matrix anti-interference ability and excellent enrichment and purification performance. The solid-phase extraction column using the nanoparticles realizes high-efficiency extraction of organophosphorus pesticide. DETAILED DESCRIPTION - INDEPENDENT CLAIMS are included for the following: (1) a solid phase extraction column, which comprises the three-dimensional graphene material modified with zirconium dioxide nanoparticles used as a filling material, which is filled between upper and lower sieve plates of the empty solid phase extraction column; and (2) detection of organophosphorus pesticide.