A new nickel/nickel boride-based nanosorbent which provides high sorption efficiency for tin(IV) was developed in this study. The sorbent capacity was found to be 26.33 +/- 2.18mg tin(IV)/g sorbent (n=3). Tin(IV) can be determined by measuring the fluorescence signal of the tin(IV)-flavonol complex. Recovery of tin(IV) with 1mol/L hydrochloric acid was found to be 98.70 +/- 1.29 (n=5). The limit of detection and the limit of quantification of the method were found to be 0.5 and 1.7 mu g/L, respectively. The calibration graph was linear in the range of 4-80 mu g/L. The adsorption type was determined by using the adsorption isotherms. Interference effects of several metal ions on tin(IV) determination were investigated and the tolerable concentration limits of these metal ions were determined. The nickel/nickel boride nanosorbent reduces the interference effects and improves the sensitivity and the selectivity of the method. With the aid of the novel nanosorbent, higher tolerable concentration limits of interfering ions like molybdenum(VI), phosphate, and fluoride compared to the standard detection method were observed in this study. The proposed method was applied to canned tomato paste and canned corn. The novel nickel-nickel boride sorbent appears to be one of the sorbents with high capacity and enrichment factor. Characterization of the sorbent was investigated.