Macaroni products are hydrolyzed in concentrated HCl (1 + 1) and saponified by the addition of KOH pellets. Aqueous layer containing soaps is separated, and ether layer is washed several times with dilute KOH. Ether is slightly acidified, filtered, and dried, and residue weight is corrected by reagent blank. Residue is reported as % unsaponifiable matter. This method is applicable to macaroni and other extruded pasta products.