A simple and efficient procedure was developed to determine eight herbicides in corn flour by gas chromatography -mass spectrometry in selected ion monitoring mode. Samples were prepared with a modified quick, easy, rapid, effective, rugged, and safe procedure. The type and volume of extraction solvent, type and amount of adsorbent, and time of sonication were optimized. The protocol method was rigorously verified. The mean recoveries were from 85 to 108% at various fortification levels with relative standard deviations below 15% and limits of quantification from 4 to 48 ng/g. The method was employed to determine herbicides in corn flour.