The objectives of this study were to optimize instrumental parameters and conditions for analysis of selected organophosphorus pesticides (OPPs) by gas chromatography (GC) with nitrogen-phosphorus detection (NPD) (GC-NPD); to select an appropriate solvent system; to conduct a comparison of sonication and shaking extractions; and to select an appropriate procedure for extracting organophosphorus pesticides from soils. Procedure Ⅰ consisted of n-hexane or petroleum ether together with acetone used as solvents, while Procedure Ⅱ contained several solvents including acetone,methanol, dichloromethane, and n-hexane or petroleum ether. Experimental results indicated that a mixture of petroleum ether/acetone (2:1, v/v) could be used in place of n-hexane/acetone (2:1, v/v) as it was a less expensive solvent system.In addition, shaking under a water bath at 20 ℃ was more effective than sonication. Also, Procedure Ⅰ was more effective,safer, and more timesaving than Procedure Ⅱ. Procedure I was applied to three soil types of different organic matter content, with recoveries of the OPPs from the yellow-brown soils, which had a higher organic matter content, being lower than those from the yellow and red soils.