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A simple rapid analytical method for determining the concentration of ZnO nanoparticles in aqueous dispersion has been developed by adding porphyrin (TCPP) as a fluorophore into the water sample for fluorescence analysis. Quenching of the emission intensity at 650 nm provides a Stern-Volmer plot with adequate sensitivity for the detection of ZnO nanoparticles from 0.15 mg/mL up to 1.5 mg/mL. A new emission peak at 605 nm can be attributed to the formation of a unique ZnO-TCPP complex. This unique emission peak is good for both identification and quantitation of ZnO nanoparticles at low concentrations down to 0.0015 mg/mL. The new method affords a linear dynamic range up to 1.2 mg/mL.