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The increasing production of zinc oxide nanoparticles and their use in products of sanitary interest make the analysis and characterization extremely important from the point of view of public health and environmental risk. This work aimed to validate the methodology using SP-ICP-MS to measure and quantify nanoparticles of ZnONPs and dissolved zinc—Zn(i). This study pointed out that the method was suitable for the purpose, presenting satisfactory results for the recovery and precision test for Zn(i) and size of NPs. The limits of detection size, dissolved zinc concentration, and particle concentration were 67 nm, 0.4 µg L−1, and 1.08 × 105 particles mL−1, respectively. Thus, the results obtained demonstrate that the technique can be used to determine the size and concentration of Zn(i) in different products. [ABSTRACT FROM AUTHOR]