The occurrence of glucosinolates within particular plant families, notably the Cruciferae, is responsible for a pungent taste, as on crushing hydrolysis takes places. This autolysis brought about by contact of glucosinolates and the endogenous enzyme system, yields one or more of the following: isothiocyanate, nitrile, thiocyanate, cyanoepithiobutane, oxazolidinethione or thionocarbamate, along with glucose. Various workers have employed chromatographic separation techniques including paper, thin-layer and gas chromatography (GC) for characterisation of the aglucone autolysis products. Owing to the volatility of most of these products and the resolution of GC, this latter method is frequently employed. Both packed and capillary columns have been used for separating the products and retention data and mass spectrometry used for identification. Previously used autolysis protocols involve treatment of large amounts of plant material (from 250 mg to whole plants) followed by defatting, then solvent extraction or distillation of the aglucones. In order to determine the glucosinolates and their degradation products elaborated by plant cell cultures of the Cruciferae, we required a very sensitive method applicable to small sample sizes. Using material from Descurainia sophia and Alyssum minimum we decided to check a range of extraction procedures for qualitative and quantitative differences in the derived glucosinolate degradation products. Except one report of allylisothiocyanate in seeds of Sisymbrium sophia (presently known as Descurainia sophia) there are no previous mentions of isothiocyanates in either of these two plants.