The work presents the preparation of spent brewer’s yeast β-glucans by chemical and thermic treatment of yeast cell wall with NaOH solution at different temperatures. The yeast cell wall obtained by autolysis or ball milling of the brewer’s yeast was used as raw material for the preparation of β-glucans. It has been demonstrated that a single alkaline extraction using 1,0 N NaOH solution at 90 0C leads to the highest efficiency. It carried out a β-glucan product with high carbohydrate content of 88,7 %, β-glucan content of 50,4 % (w/w) and with a low protein content of 2,9 % (w/w). The β-glucan content was determined by chemical assays.