Cyanogenic glucosides were studied using Raman spectroscopy. Spectra of the crystal forms of linamarin, linustatin, neolinustatin, amygdalin, sambunigrin, and dhurrin were obtained using a Raman spectrograph microscope equipped with a 532 nm laser. The position of the signal from the C≡N triple bond of the cyanohydrin group was influenced by the nature of the side group and was above 2240 cm<sup>-1</sup> for the three cyanogenic glucosides that contain a neighboring aromatic ring, and below or partially below 2240 cm<sup>-1</sup> for the non-aromatic cyanoglucosides. Signals from the CN bond of linamarin/lotaustralin in leaves and roots from a medium cyanogenic cassava variety were obtained <i>in situ</i> using a Fourier transform near-infrared (FT-NIR) Raman interferometer with a 1064 nm laser, but the signal was very weak and difficult to obtain. A spectrum containing a signal from the CN bond of dhurrin in a freeze-dried sorghum leaf was also obtained using this instrument. Surface-enhanced Raman Spectroscopy (SERS) was demonstrated to be a more sensitive method that enabled determination of the cyanogenic potential of plant tissue. The SERS method was optimized by flow injection (FI) using a colloidal gold dispersion as effluent. Potential problems and pitfalls of the method are discussed.

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