A specific, sensitive and quantitative method for measuring tissue sulfhydryl (SH) and disulfide levels in nonprotein, protein, and protein-bound fraction has been developed by using HPLC with electrochemical detection. Protein and nonprotein fractions are separated through perchloric acid precipitation. The protein fraction is divided into two aliquots: one which undergoes protein hydrolysis in HCl and the other which undergoes sodium borohydride reduction. The nonprotein, protein and protein-bound fractions generated are then separated by HPLC and the various sulfhydryls (e. g. , cysteine, glutathione) and disulfides (e. g. , cystine, glutathione disulfide) are measured directly by a dual gold mercury electrode thin layer electrochemical cell.