Acrylamide (AAm) is classified as a potential carcinogen and neurotoxin because of its neurotoxicity, reproductive toxicity, genotoxicity and immunotoxicity. The cooking of some carbohydrates-rich food at high temperature increases the high risk for exposure to AAm. It is of great significance and practical value to establish a rapid analytical method for acrylamide. Surface-enhanced Raman scattering (SERS) technique has been developed rapidly in recent years. Based on the highly active SERS substrate, the identification of the fingerprint of compound can be realized. To achieve the rapid SERS analysis of the target substance in the complex substrate, a highly active enhanced substrate and an efficient sample pretreatment technique were required. A rapid, reliable, and quantitative method to determine acrylamide content in fried food based on Ag nanorod/Au nanoparticle composites (AgNR@AuNPs) SERS has been proposed. Based on the enhanced effect of double “hot spots” between AgNR nanorods and AuNPs nanoparticles, the substrate has a high SERS enhanced activity for acrylamide. Besides, AgNR was a solid phase substrate. Before each operation, the oxide on the surface was removed by dilute nitric acid, which greatly improved the stability of SERS analysis. The size of AuNPs and the testing sequence which influence the sensitivity of SERS detection have also been investigated. The fried food was complicated with lots of interferences. The dispersive solid-phase extraction was used for decreasing the serious interference of complex matrix. The defatting and extraction solvent, the kind and ratio of cleanup material have been optimized. The results have shown that the optimized defatting solvent, the extraction solvent and the cleanup materials were hexane, the mixture of water and acetonitrile (1∶1, V/V), and MgSO4+NaClrespectively. The total detection time approximately costed was within 5 min with the limits of detection as low as 1 μg·kg-1 based on the quick pretreatment and SERS enhancement. The peak at Δν=1 482 cm-1 was selected as the characteristic peak of acrylamide for quantitation in the concentration range of 5～100 μg·kg-1 (r=0.985). The recovery rates for acrylamide were 77.1%～93.6% with coefficients of variation less than 4.0% at five different fortified concentrations. The developed method can potentially be used for acrylamide detection in the field.