Currently, one of the significant environmental problems is the presence of azo dye materials in water sources. In this study, for the first time, a fast and sensitive sample preparation approach using nanoparticle-assisted fabric phase sorptive extraction (NFPSE) followed by high-performance liquid chromatography was examined to remove some azo dyes such as methyl red and sunset yellow from aqueous solutions. Primarily, the significance of several parameters affecting NFPSE, such as fabric type, the kind of sorbent, the number of contacts with sol-gel and the time of contact, was investigated. In addition, experiments were performed to determine the effect of different adsorption parameters, such as sample volume, adsorption time, adsorbent value, desorption time, ionic strength and pH. It was found that the calibration curve was linear within two ranges of concentrations (0.05-0.1 and 0.5-15ng/L for methyl red; 0.05-0.5 and 0.5-15ng/L for sunset yellow) with correlation coefficients better than 0.9683. The limit of detection was 0.014ng/L for methyl red and 0.015ng/L for sunset yellow. Repeatability Relative Standard Deviation (RSD) with three replicated experiments was 1.5-10% for methyl red and 2.5-5.8% for sunset yellow. Relative recovery percentages of 88-96% for methyl red and 62-92% for sunset yellow were obtained in the samples. Moreover, the results have shown that acceptable accuracy, precision and linearity make the "fabric phase sorptive extraction" a proper method for the determination of dyes from industrial sewage samples.