1. A method is described for the quantitative separation of the sulphur compounds in a single sample of tissue by passing an extract through a serial assembly of ion-exchange resins in the order: Dowex 2 (Cl− form), Dowex 1 (CO32− form), Amberlite CG-50 (H+ form) and Zeo-Karb 225 (H+ form). 2. Groups of sulphur amino acids were eluted separately from each column; the recovery of sulphur compounds after their labelling with 35S in vivo by injection of l-[35S]-methionine was 91–106%. Individual sulphur compounds were further resolved by one-dimensional or two-dimensional paper chromatography. 3. Evidence is presented on the occurrence of S-adenosylmethionine and S-adenosylhomocysteine in rat liver and brain. Rat liver and brain contained 83·6 and 31·4mμ-moles/g. respectively of S-adenosylmethionine.
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