Nanotechnology offers substantial prospects for the development of state-of-the-art products and applications for agriculture, water treatment, and food industry. Profuse use of nanoproducts will bring potential benefits to farmers, the food industry, and consumers, equally. However, after end-user applications, these products and residues will find their way into the environment. Therefore, discharged nanomaterials (NMs) need to be identified and quantified to determine their ecotoxicity and the levels of exposure. Detection and characterization of NMs and their residues in the environment, particularly in food and agricultural products, have been limited, as no single technique or method is suitable to identify and quantify NMs. In this review, we have discussed the available literature concerning detection, characterization, and measurement techniques for NMs in food and agricultural matrices, which include chromatography, flow field fractionation, electron microscopy, light scattering, and autofluorescence techniques, among others.