The charcoal trap adsorption device was designed and used to adsorb the volatile organic compounds (VOCs) emitted from Ginkgo leaves and Lima beans. The adsorbed VOCs were determined using gas chromatography-mass spectrometry (GC-MS). Compared to solid phase microextraction (SPME), the self-made charcoal trap adsorption device was more advantageous to the enrichment of VOCs from Ginkgo leaves. Additionally, the quantitative analysis of the collected VOCs released from Lima beans was carried out through the addition of internal standard, and the results of the two parallel experiments showed good repeatability. Because the eluent of the charcoal trap can be stored and used in the quantitative analysis as well as parallel experiments, the self-made charcoal trap adsorption device coupled with GC-MS is suitable for laboratory studies of plant volatile organic compounds.