Use of Closed-System Vacuum Distillation for Isolation of Moderately Volatile Compounds
Abstract A rapid, efficient vacuum distillation method has been used to quantitatively determine moderately volatile compounds in food-related samples. The following components and matrices were studied: 1,4-dioxane in polysorbate 65 and choline chloride; ethylene chlorohydrin in choline chloride, choline bitartrate, and cumin; and epichlorohydrin, 1,3-dichloro-2-propanol, and l-chloro-2-propanol in cornstarch. The matrix is slurried with water or aqueous methanol, frozen, and subjected to vacuum distillation. The distillate, which is free of salts and nonvolatile matrix components, is chromatographed on a gas chromatographic column and quantitated using a flame ionization detector. Foaming, which is a problem with purge and trap and azeotropic distillation procedures, does not occur. Recoveries of the components ranged from 85 to 101% at levels of 0.5-600 ppm