Allylisothiocyanate is determined spectrophotometrically after reaction with 2,3-dichloro-1,4-naphthoquinone. For pure samples, the color intensity is proportional to allylisothiocyanate content in the range 0.8-3.0 mg/ml reaction mixture. A modified procedure is used to estimate allylisothiocyanate content of mustard seed oil. The reaction is linear for allylisothiocyanate concentrations in the range 40-240 mug/ml reaction mixture. Two mustard seed oil samples contained 0.995 not equal to 0.020 and 0.981 not equal to 0.019% allylisothiocyanate.