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Plants emit volatile organic compounds (VOCs) from various organs. To understand the biological and ecological roles of plant VOCs as well as their biosynthesis, it is important to determine the quality and quantity of individual plant VOCs. Here we describe three techniques, including solid-phase microextraction, closed-loop stripping system, and an open dynamic system, for sampling volatiles emitted from insect-damaged rice plants. In addition, the protocol for using gas chromatography-mass spectrometry to elucidate the chemical identities of rice volatiles is described.