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J Assoc Off Anal Chem. 1987 Mar-Apr;70(2):215-26.

Purge and trap method for determination of volatile halocarbons and carbon disulfide in table-ready foods.


A method developed for the determination of ethylene dibromide in table-ready foods has been modified and expanded to include 7 other volatile halocarbons and carbon disulfide. Samples are stirred with water and purged with nitrogen for 0.5 h in a water bath at 100 degrees C. The analytes collected on a duplex trap composed of Tenax TA and XAD-4 resin are eluted with hexane and determined by gas chromatography with electron capture detection or Hall electrolytic conductivity detection. Flame photometric detection in the sulfur mode is used to determine carbon disulfide. Thick-film, wide-bore capillary columns are used exclusively in both the determination and confirmation of the halogenated analytes. The higher levels of analytes are also confirmed by full scan gas chromatography mass spectrometry (GC/MS). Samples are analyzed for carbon disulfide, methylene chloride, chloroform, 1,2-dichloroethane, methyl chloroform, carbon tetrachloride, trichloroethylene, 1,2-dibromoethane, and tetrachloroethylene. Initially, 19 table-ready foods from the Food and Drug Administration's Total Diet Study were analyzed by this method. A limited survey of those food items exhibiting high levels of analytes was conducted. Samples exhibited levels up to 3300 ppb (methyl chloroform in Parmesan cheese). Recoveries of all 9 analytes from fortified samples ranged from 83 to 104%. Chromatograms from this purge and trap method are clean, enabling quantitation levels of low parts per billion and sub-parts per billion to be achieved for the halogenated analytes. The quantitation limit for carbon disulfide is 12 ppb. Two compounds found in drinking water were identified by GC/MS as bromodichloromethane and chlorodibromomethane. Drinking water from several cities was analyzed for these trihalomethanes as well as for bromoform. Levels of up to 17 ppb bromodichloromethane were found. Recoveries ranged from 96 to 103%.

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