This chapter describes the use of molecular vibrational spectroscopy to assess the quality and safety of agro-food products. Molecular vibrational spectroscopy refers to the measurement of radiation intensity as a function of frequency (expressed as a function of wavenumber or wavelength) in the 12,800-50 cm−1 range (or 780-200,000 nm) of the electromagnetic spectrum, which relates mainly to characteristic molecular vibrations. In order to perform this measurement, spectrometers (also called spectrophotometers) are used to acquire the spectra of absorbance resulting from the interaction of the radiation with all the constituents of a product, as well as their physical state. In the past two decades, the application of molecular vibrational spectroscopy techniques to solve analytical problems has continued to increase, with a major focus in the agro-food industry being on the routine control and monitoring (inline and online analysis) of quality, nutritional, and technological parameters. The chapter reects the renewed interest in the use of molecular vibrational spectroscopy techniques for addressing emerging food safety issues at both the industry and laboratory levels. The techniques are important for risk managers seeking to tackle the source of problems before these problems enter the food chain and contaminate links within it.