Solid phase microextraction (SPME) is used to collect and concentrate the compounds in the headspace of rice. This research describes optimization parameters of temperature, moisture, and sampling time. Optimization was based upon the recovered levels of 2-acetyl-1-pyrroline (2-AP), the popcorn aroma in aromatic rice. The method uses a sampling temperature of 80 degrees C and adds 100 microL of water to a 0.75 g sample of rice. The rice was preheated for 25 min, a carboxen/DVB/PDMS SPME fiber was exposed to the headspace for 15 min, and a subsequent GC-MS analysis took 35 min. Samples of rice can be analyzed as the flour, milled kernels, or brown rice. Twenty-one experimental rice varieties were analyzed by the SPME method and compared to a wet technique. Recoveries of several nanograms of 2-AP from 0.75 g samples of aromatic rice were observed, whereas only trace amounts of 2-AP were recovered from nonaromatic rice. Recovery from a single SPME headspace analysis is calculated to be 0.3% of the total 2-AP in the sample.