Bioactive organosulfur phytochemicals were isolated from fresh broccoli using methlylene chloride as an extract solvent and identified by GC/MSD analyses. Major organosulfur phytochemicals of broccoli extract were found to be isothiocyanates, which constitute 40.42% of total phytochemicals. The isothiocyanates from broccoli extract were identified to be 3-butenyl, 4-methyl thiobutyl, 4-methylthio-3-butenyl, 5-methylthiopentyl, 2-phenylethyl, 3-methyl sulfinyl propyl, and 4-methylsulfinylbutyl isothiocyanates, of which major isothio cyanates were 3 butenyl isothiocyanate and 4-methylsulfinylbutyl isothiocyanate, constituting about 38.55% of total isothiocyanates present in the solvent extract. Also, nitrites, corresponding to products from enzymatic hydrolysis of glucosinolates were identified as 4-methylthiobutyl, 5-methyl thiopentyl, 2-phenylethyl and 4-methylsulfinylbutyl nitrile. In addition, three sulfides were identified as dimethyl disulfide, dimethyl trisulfide and dimethyl tetrasulfide.