The amounts of dimethyl disulfide and dimethyl trisulfide decreased as sample holding time in an autosampler (4 °C) before purge increased, whereas those of aldehdyes increased as holding time increased due to lipid oxidation. Helium flush of sample vials before sample loading on an autosampler retarded lipid oxidation and minimized the changes of sulfur volatiles in raw meat, but was not enough to prevent oxidative changes in cooked meat. Although DH/GC-MS is a powerful method for automatic analysis of volatiles in meat samples, the number of samples that can be loaded in an autosampler at a time should be limited within the range that can permit reasonable repeatabilities for target volatile compounds.