Methyl bromide (MB, bromomethane) is determined in a variety of foods by headspace capillary gas chromatography with electron capture detection. The comminuted food sample as an aqueous sodium sulfate slurry is equilibrated with stirring for 1 h at room temperature before a 1 mL headspace aliquot is removed and injected using a modified on-column syringe needle. Methyl bromide is cryogenically focussed at -60 degrees C and then eluted by temperature programming. The procedure requires blending of soft samples, e.g. raisins, prunes, or oranges, and ultrasonic homogenization of hard samples, e.g. wheat, cocoa beans, corn, or nuts, with portions of water and ice so the final temperature of the food-water slurry is less than 1 degree C. A 20 g aliquot (4 g food) is then added to a cold headspace vial containing 4 g sodium sulfate. Losses of MB during a 3.5 min ultrasonic homogenization of wheat were 11% at 0.95 ppb and 4.4% at 4.8 ppb. For flour, cocoa, and finely divided spices, which do not require blending, 4 g is added to the cold headspace vial containing 16 mL cold water and 4 g sodium sulfate. Studies show that comminution of wheat or peanuts must be carried out to release MB trapped within the food so the headspace equilibrium can be attained in 1 h as well as to obtain homogeneous samples and representative sampling. No interferences were noted with the above foods or with many grain-based baking mixes analyzed.(ABSTRACT TRUNCATED AT 250 WORDS)