Abstract: The effects of extraction temperature, equilibration time, extraction time and resolution time for headspace solid-phase microextraction(HS−SPME) on the extraction of volatile organic compounds(VOCs) of Eucalyptus particleboard were investigated by single factor experiment combined with gas chromatography-mass spectrometry(GC−MS) analyses, and the extraction condition were optimized by using response surface methodology. The results showed that the extraction time and temperature showed remarkable effect on VOCs extraction, and the optimal extraction parameters were 91℃ of extraction temperature, 34 min of equilibration time, 24 min of extraction time and 2.5 min of resolution time. Under this optimal condition, the relative error between the validation test results and the predicted value was 0.62%, and a total of 54 VOCs including 23 olefins, 11 alcohols, 8 alkanes, 5 aromatic hydrocarbons, 5 aldehydes, 1 ester and 1 acid were detected from Eucalyptus particleboard. The results will provide a basis for the further detection and analysis of the VOCs in Eucalyptus particleboard.