A method for the rapid determination of ethyl carbamate in wine by headspace solid-phase microextraction with detection by gas chromatography/mass spectrometry has been developed. The analysis parameters of fiber coating, extraction time, and sample temperature have been optimized. The optimized method of headspace sampling with a Carbowax/divinylbenzene fiber for 30 minutes has been found to be reproducible and linear from 10 to 80 mug/L, with a limit of detection of 9.6 mug/L. The method is simple, requires little operator effort, and can be automated.