Gas-liquid chromatographic-mass fragmentographic determination of low levels of diethylcarbonate in beverages.
Sodium chloride and ethanol (omitted for samples with greater than 10% alcohol) are added to the beverage sample and the sample is allowed to equilibrate in a 30 degrees C water bath. An aliquot of the headspace is injected into a gas chromatography containing a column packed with 0.2% Carbowax 1500 on 80--100 mesh Carbopack C. During the elution of diethylcarbonate (DEC), an impurity that is present in diethylpyrocarbonate, the column effluent is vented to a mass spectrometer with a multiple ion detection system and operated in the electron impact mode. The ions at m/e 63 and 91 are monitored. Lemonade, fruit drinks, wine, and beer samples (138 total) were analyzed for DEC. Sixteen samples had greater than 30 ppb DEC. Eight analyses of a lemonade sample gave a mean of 88 ppb with a coefficient of variation of 11%.
D001628:Beverages / Q000032:analysis*; D004047:Diethyl Pyrocarbonate / Q000031:analogs & derivatives / Q000032:analysis*; D005503:Food Additives / Q000032:analysis; D005561:Formates / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry
D005503:Food Additives; D005561:Formates; D004047:Diethyl Pyrocarbonate