To develop a rapid, accurate and sensitive method for the simultaneous determination of five industrial dyes (acid red 2G, acid red 14, acid yellow 73, orange 2 and acid blue 62) by solid phase extraction (SPE) and high performance liquid chromatography.Methods Samples were extracted by ammonia-methanol-water (2∶18,V/V), and cleaned up by the HLB solid phase extraction column. The analytes were washed with 0.1% formic acid, eluted with 5% ammonia-methanol and dried by nitrogen. The residue was dissolved with the initial mobile phase, and the solution was separated on a ZORBAX SB-C₁₈(4.6 mm×250 mm, 5μm)column by using acetonitrile-ammonium acetate solution as the mobile phase in gradient program. Detection was performed with UV detector of variable wave-length. Quantitative analysis was carried out by measuring peak area and comparing it with external standard. Results There was good linearity in the range of 0.50-50 mg/L for the five dyes. Recoveries were in the range of 86.0%-110.2%, and the relative standard deviation (RSDs) were lower than 6%. The limits of quantification (LOQs) were in the range of 0.5 mg/kg. Conclusion This method is simple, sensitive and reproducible, which could be applied to the routine analysis.