Gas-liquid chromatographic-mass fragmentographic determination of low levels of diethylcarbonate in beverages

• Published in: Journal of the Association of Official Analytical Chemists Vol. 62; no. 2; p. 253
• Main Authors: van Lierop, B H, Nootenboom, H
• Format: Journal Article
• Language: English
• Published: United States 01.03.1979
• Subjects: Beverages - analysis; Diethyl Pyrocarbonate - analogs & derivatives; Diethyl Pyrocarbonate - analysis; Food Additives - analysis; Formates - analysis; Gas Chromatography-Mass Spectrometry
• ISSN: 0004-5756
• DOI: 10.1093/jaoac/62.2.253

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%.