Abstract: As a new preparation technique, solid-phase microextraction(SPME) focus sampling, extraction, concentrating and desorption in one simple step. SPME is a solvent-free, rapid, inexpensive and field usable technique, in which analytes are adsorbed from an aqueous sample onto a phase-coated fused silica fiber. The fiber is then inserted directly into the GC injection port for thermal desorption. SPME is combined with GC for determination of trace volatile organic compounds in packing films, including isopropanol, ethyl acetate, butanone and toluene. Linear rang is found to be more than 10² level. Limits of detection are below 4.44 ng/mL and the precision are from 2.3%～4.7%. The method has higher sensitivity and better repeatability.