气相-质谱法测定粮谷中恶草酮的残留量

 应用微量化学法和固相萃取技术 ,建立了粮谷中恶草酮残留量的气相 质谱 (GC MS)测定方法。用苯 正己烷 (体积比为 1∶1)萃取 ,中性氧化铝小柱净化。净化液用GC MS测定 ,采用外标法定量。恶草酮在大米中的回收率为 90 4%～ 115 .7% ,RSD为 2 %～ 6 % ,在玉米中的回收率为 81 3%～ 10 9 7% ,RSD为 4%～ 9% ,最低定量检出限为 0 0 0 5mg/kg。该法快速、灵敏、准确 ,各项技术指标均满足农药残留检测的要求。

Determination of Oxadiazon Residues in Cereals by Gas Chromatography-Mass Spectrometry

An efficient method with microchemical method and solid phase extraction (SPE) technique for the determination of oxadiazon residues in cereals by gas chromatography-mass spectrometry (GC-MS) has been established. The oxadiazon was extracted from the sample with benzene-hexane(1:1, V/V). The extract was cleaned-up by a column of 500 mg Supelclean LC-Alumina-N. When the blank rice and corn were spiked with oxadiazon in the range of 0.005 mg/kg-5.00 mg/kg, the recoveries were 90.4%-115.7% for rice and 81.3-109.7% for corn, and with RSD of 2%-6% and 4%-9% respectively. The limit of detection was 0.005 mg/kg. The method is rapid, sensitive, accurate and suitable for the analysis of pesticide residues.