Large quantities of volatile organic compounds (VOCs) are released from heat-treated bamboo during the manufacturing process of recombinant bamboo, which affects the environment and human health. In this study, bamboo was treated at 150 °C, 180 °C, and 210 °C for 3 h, and VOCs were collected every hour using a Tenax tube. The VOCs were analyzed with gas chromatography-mass spectrometry (GC-MS) to explore the effect of temperature and time on weight loss ratio, main components, and their relative proportions. The results showed that temperature considerably influenced weight loss ratio, and weight loss ratio increased rapidly at high temperature. Massive quantities of VOC were emitted during the first hour of treatment, and emissions decreased as the time and temperature increased. Terpenes were the primary component of the VOC emissions. Temperature and time exhibited minimal effects on the type of primary components, and the relative proportion of some components exhibited negligible changes over a range of temperatures and times.