采用固相萃取气相色谱–质谱法同时检测水体中的微量对硫磷和甲基对硫磷.水样用固相萃取柱进行富集,以丙酮洗脱,经气相色谱–质谱仪进行定性定量分析.对硫磷、甲基对硫磷的质量浓度在0.01～1.0μg/mL范围内与其色谱峰面积均呈良好的线性关系,线性相关系数不小于0.995,检出限分别为0.004,0.002μg/mL.对硫磷、甲基对硫磷测定结果的相对标准偏差均小于5％(n=6),重复性小于10％(n=6),加标回收率在82.2％～90.5％之间.该方法检测速度快,灵敏度度高,可用于水体中微量对硫磷和甲基对硫磷的检测.%A solid phase extraction gas chromatography–mass spectrometry method for determination of microscale parathion and parathion-methyl residuals in water was established. After being enriched by solid phase extraction column and eluted with acetone, the samples were determinated qualitatively and quantitatively by gas chromatography–mass spectrometer. The concentration of parathion and parathion-methyl was linear with its chromatographic peak area in the range of 0.01–1.0 μg/mL, the correlation coefficients were more than 0.995. The detection limits of parathion and parathion-methyl were 0.004, 0.002 μg/mL,respectively. The relative standard deviations of detection results of parathion and parathion-methyl were less than 5％(n=6),and the repeatability was less than 10％(n=6). The addtion recoveries ranged from 82.2％ to 90.5％. This method is quick to operate,has good sensibility, it can be used to determine microscale parathion and parathion-methyl residuals in water.
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