In this paper, the carbon nanotubes (CNTs) solid phase microextraction (SPME) probe was prepared and characterized. The octylphenol and nonylphenol in the water were determined by the probe coupled with the GC-MS method. The factors which impact extraction efficiency such as extraction temperature, extraction time, sample dilution multiple and ionic strength were optimized. A pulse stress of carrier gas was applied to the inlet of GC column to improve the determination sensitivity of GC-MS. The method linear ranges of octylphenol and nonylphenol were from 0.01μg·L-1 to 20μg·L-1, and the related coefficient was 0.992 and 0.996. The recoveries were from 91.89% to 92.01%, detection limits were from 0.01μg·L-1 to 0.02μg·L-1, and relative standard deviations (RSDs) were from 3.2% (n=5) to 4.1% (n=5).