A new magnetic nano gel (MNG) was prepared from choline chloride/phenol deep eutectic solvent and magnetic amberlite XAD-7 nanocomposite. The dispersive solid phase micro extraction (dSPME) method was developed for seperation and preconcentration of Brilliant Blue FCF (BB) by the prepared MNG. In this study, firstly, the optimum DES type and mole ratio of DES were investigated before response surface methodology optimization. Then, the effect of the MNG-dSPME experimental parameters were optimized by response surface methodology using central composite design. Under the optimum microextraction conditions, limit of detection (LOD), limit of quantification (LOQ), preconcentration factor (PF), enhencament factor (EF) were found to be 1.15 μg L−1,3.80 µg L-1, 70, and 88, respectively. It was seen that the recovery of real samples were obtained from 95.5 to 103.6%. The pesent method was succesfully for extraction of BB in some food, personal care samples, to the best of our knowledge, this is the first study that is presented method on determination of BB by preconcentration with magnetic nano gel. The obtained results showed that the present procedure is effective, sensitive, and has high accuracy for the quantitative detection of BB.