Magnetic solid phase extraction (MSPE) accompanied with fluorescence spectrophotometry using Poly (ionic liquid) immobilized magnetic nanoparticles (PIL-MNPs) as sorbent was introduced for Congo red analysis in food. Poly (1-vinyl-3-butylimidazolium) bromide immobilized (MNPs) were prepared through co-polymerization of 1-vinyl-3-hexylimidazolium-based ionic liquid and vinyl-modified magnetic particles. Some of different types of parameters, such as pH value, adsorption temperature and time, sample volume, eluent type, were studied. Under the optimum conditions, the preconcentration factor for AR was 27. The linear range, detection limit (DL), correlation coefficient (R) and relative standard deviation (RSD) were found to be 0.10-9.00µg/mL, 5.2µg/L, 0.9987 and 3.10% (n=3, c=4.00µg/mL). This method had been successfully applied to the separation / analysis of Congo red in real samples.