AbstractA simple and sensitive method for the quantitative determination of volatile isothiocyanates in canola oil has been developed. The method is based on the specific absorbance of isothiocyanates in the infrared region. The results obtained were confirmed by gas liquid chromatography using a flame photometric detector. The various volatile isothiocyanates isolated from the oil were allyl isothiocyanate, 3‐butenyl isothiocyanate, 4‐pentenyl isothiocyanate and 2‐phenethyl isothiocyanate. Their identities were confirmed by mass spectroscopy and by retention times. The recoveries of sulfur from volatile sulfur compounds by this method ranged from 93.6% to 101.1% when compared to the amount determined by gas liquid chromatography. The coefficients of variability of volatile sulfur compounds in canola oils ranged from 1.7% to 3.2%. The sulfur content represented by the volatile sulfur compounds comprised 21.7% of the sulfur determined by the Raney nickel method for crude oil, 36.6% for refined oil and 22.7% for refined, bleached and deodorized oil.