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福建水产 ›› 2012, Vol. 34 ›› Issue (6): 466-470.

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法测定海水及水产品中的莠去津

吴茂生   

  1. 福建省海洋环境与渔业资源监测中心
  • 收稿日期:2012-08-23 修回日期:2012-10-09 出版日期:2012-12-25 发布日期:2012-12-20
  • 通讯作者: 吴茂生

Determination of Atrazine in seawater and sea food by Gas Chromatohraph-Mass Spectrum

  • Received:2012-08-23 Revised:2012-10-09 Online:2012-12-25 Published:2012-12-20

摘要: 本文采用有机溶剂萃取的提取方法,利用气相色谱-质谱选择离子检测,建立了海水及水产品中莠去津的检测方法。该方法在0.001~0.5 ug/L的范围内具有良好的线性范围,线性相关系数为0.9996;在海水和水产品中检出限(S/N=3)分别为0. 001 μg/L和0. 001 mg/kg;在加标回收率试验中,海水中莠去津回收率为95.8%~113.2%,水产品中莠去津回收率为83.1%~92.6%;相对标准偏差(n=6)均小于4.4%。

关键词: 气相色谱-质谱, 莠去津, 海水, 水产品, Gas chromatohraph-mass spectrum, atrazine, seawater, sea food

Abstract: A gas chromatohraph-mass spectrum method was established for determination of the atrzine in seawater and sea food. The pretreatment and chromatographic conditions were optimized. The total of 50 mL dichloromethane was chosen in the process of organic solvent-seawater extract with liquid-liquid extraction technique. Florisil SPE column and hexane mixed with ethyl acetate were used to clean up the sea food sample so as to reduce continuum organic interference in GC-MS detection. Identification was achieved by Electron Ionization mode ( EI ) using select ion monitoring (SIM). Under the optimal conditions,good linearities were obtained for atrazine in the range of 0.001~0.5 ug/L. The quantification was performed with internal standards. The recoveries of atrazine in seawater and sea food were in the range of 95.8%~113.2% and 83.1%~92.6% respectively. The relative standard deviations (RSD) were less than 4.4%. The limits of detection were 0.001 μg/L for atrazine in seawater, and 0.001 mg/kg for atrazine in sea food. The method has been successfully applied to determination of atrazine in seawater and sea food in sea area of Fujian Province during an accident.