The invention discloses a preparation technology of a nano-Fe3O4-V2O5-Au-doped poly-naphthylamine film modified netted glassy carbon electrode. The technology comprises dissolving FeCl3 and NaAc in glycol, drying to obtain particles A; mixing cetyl trimethyl ammonium bromide, n-octane and n-butanol, dividing into two parts, adding ammonium metavanadate and deionized water into one part, stirring to obtain a microemulsion A, adding dilute sulfuric acid into the other part, stirring to obtain a microemulsion B; mixing the microemulsion A and the microemulsion B, centrifuging, washing, roasting to obtain particles B; mixing the particles A and the particles B, adding polyvinyl pyrrolidone, an HAuCl4 solution and the deionized water, shaking and centrifuging, adding washed and dried product, sodium dodecyl benzene sulfonate and naphthylamines into the deionized water and mixing, adding ammonium persulfate, shaking and centrifuging, dissolving the washed product into acetone, adding pre-treated netted glassy carbon, shaking, taking the product out, and drying to obtain the nano-Fe3O4-V2O5-Au-doped poly-naphthylamine film modified netted glassy carbon electrode.