In order to rapidly determine deoxynivalenol (DON) and Zearalenone (ZEN) in maize, a rapid quantitative immunofluorescence assay based on superconductor coating was used to detect multiple maize samples. Combined with the recovery rate, stability, detection limit, precision and other indexes, the applicability of the method was evaluated and compared with the results of liquid chromatography. The results showed that the superconductor coated immunofluorescence diaper method had the good linearity in the range of 100 ng/mL~2 500 ng/mL for DON and 5~200 µg/kg for ZEN. The recoveries of DON were 103.72%~108.17% in the range of 500~2 000 µg/kg, and 97.81%~111.27% in the range of ZEN 50~150 µg/kg. Compared with the results of liquid chromatography, the superconductor coated immunofluorescence diaper method is an effective, practical, rapid and quantitative analysis method within the allowable deviation range, which can meet the requirements of simultaneous detection of DON and ZEN in maize.