A serious problem in analyzing pesticide residues in foods by gas chromatography/mass spectrometry (GC/MS) is the matrix enhancement e ect. e matrix e ect of pesticides in 5 types of representative samples preprocessed by the Positive List System was measured at 100 ppb. e mean matrix e ect value of pesticides in potato, spinach, orange, brown rice, and soybean sample was 129%, 191%, 171%, 225%, and 146%, respectively. Continuing research showed that the sample solutions contained high amounts of some matrix components, such as tocopherols, sterols, and monoacylglycerols. In order to investigate which component causes the matrix e ect, each matrix solution was prepared at 1-1000 ppm (monoacylglycerols: 1-500 ppm), and the pesticide mixture was forti ed to 100 ppb. e matrix e ect depended on the concentration of the matrix solution, and we concluded that monoacylglycerols were the most attributable components to the matrix e ect.