A method for the determination of prometryn in aquatic products with solid phase extraction-gas chromatography mass sepectrometry (SPE/GC-MS) was established. The prometryn in samples was extracted with acetonitrile, and the supernatant was purified by primary secondary amine (PSA) solid phase column. Then,the analyte was determined in selected ion monitoring of GC-MS. The calibration curves of prometryn showed good linearity in 2.5μg/L-40μg/L. The mean recoveries of the prometryn varied from 80%to 98%when spiked at 2, 10, 20 μg/kg, and the relative standard deviations were less than 10 %. The limit of the quantitative was 0.5μg/kg.%建立检测水产品中扑草净残留量的固相萃取-气相色谱质谱联用法。样品用乙腈提取，浓缩后经PSA固相萃取柱净化，由气质联用仪选择离子监测模式下测定。该方法条件下扑草净在2.5μg/L~40μg/L浓度范围内线性良好，对空白样品分别添加2、10、20μg/kg扑草净标准溶液，平均回收率在80%~98%，RSD小于10%，检出限为0.5μg/kg。
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