A novel fluorometric method has been developed for the determination of total protein in human serum with a new near-IR reagent as a fluorescence probe, based on the fluorescence recovery of the cyanine-CTAB system in the presence of protein. Maximum fluorescence is produced with maximum excitation and emission wave-lengths at 765 and 812 nm, respectively. Under optimal conditions, the calibration graphs are linear over the range 0.4-12.0 microg/mL for protein. The detection limit is 70 ng/mL, and the relative standard deviation of six replicate measurements is 1.14% for 6.0 microg/mL protein. The results are satisfactory.