Multilayer laminated films may contain organic solvents derived from adhesives, printing inks and so on. A headspace-GC/MS analysis method for the simultaneous determination of 30 substances such as toluene, xylene, acetone, methyl ethyl ketone, ethyl acetate, butyl acetate, methanol, ethanol, was developed. A N,N-dimethyl formamide solution containing an internal standard substance was added to the sample. After leaving overnight at room temperature, the headspace gas was analyzed by GC/MS. This method was applicable to a laminate film made of various materials. The organic solvents such as toluene, ethyl acetate, and heptane were detected from 6 out of 42 food packaging bags made from laminated film on Japanese market using this method.