Abstract: A standard adsorption tube series was prepared by diluting the mixed standard gas containing 5 volatile organic compounds (VOCs) including acetone, isopropyl alcohol, n-hexane, ethyl acetate, and benzene with nitrogen gas. The method of thermal desorption-gas chromatography-mass spectrometry was used for determination and plotting the working curve, and effects of matrices, including air, carbon dioxide, and methanol, on determination of the 5 VOCs with low, medium, and high contents were investigated. It was shown that linear relationships between values of the masses of the 5 VOCs and peak areas of the corresponding quantitative ions were kept in definite ranges, with detection limits (3S/N) in the range of 0.0300-1.00 ng, and RSDs (n=7) of the determined values in the range of 2.1%-5.7%. Except for the recovery of acetone and isopropyl alcohol with the low content in methanol matrix, which was greater than 200%, the recovery of the 5 VOCs with different contents in the 3 matrices was all within 90.0%-110%. It was speculated that the residual methanol in the detector affected the ionization of acetone and isopropyl alcohol, retention time of which was close to that of methanol, resulting in an increase in ion intensity and recovery.