Abstract GLC has been used to quantitatively measure the amount of sugar alcohols in dietetic biscuits. The total hexitol content is estimated by analysis of the trimethylsilyl ethers (TMS) and the individual hexitols are estimated as the acetate esters. An internal standard (1,4-sorbitan) was added to the biscuit during the extraction procedure. The TMS ethers were chromatographed on an SE-30 GLC column and the acetate esters were detected on a QF-l/BDS column. Recoveries of total hexitols from biscuits baked in the laboratory were 97–100%. Analyses of various commercial biscuits were also reported.