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固相微萃取与气相色谱-质谱联用测定有机磷杀虫剂的残留量

Determination of Organophosphorus Insecticide Residues by Solid Phase Microextraction Coupled with Gas Chromatography/Mass Spectrometry

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【作者】 帅琴杨薇郑岳君郑楚光

【Author】 SHUAI Qin1,2, YANG Wei2, ZHENG Yuejun2, ZHENG Chuguang1(d Technology,Wuhan 430074, China; 2. Material Science and Chemistry Engineering Faculty, China University of Geosciences, Wuhan 430074, China)

【机构】 华中科技大学煤燃烧国家重点实验室中国地质大学材料科学与化学工程学院华中科技大学煤燃烧国家重点实验室 湖北武汉430074湖北武汉430074湖北武汉430074

【摘要】 建立了固相微萃取与气相色谱 质谱(SPME GC/MS)联用测定水样中有机磷杀虫剂残留量的方法。探讨了影响SPME萃取效果的萃取头类型、萃取时间、解吸时间、离子强度等诸因素,优化了GC MS仪器条件。在优化的GC MS条件下,杀虫剂的响应值与浓度有良好的线性关系,检出限分别为敌敌畏0 40μg/L、甲基对硫磷0 01μg/L、马拉硫磷0 025μg/L、对硫磷0 004μg/L。方法用于实际水样分析,结果令人满意,样品的加标回收率为94 7%~110 0%。该方法具有分析速度快、灵敏度高、重现性好、预处理简单易行等优点。

【Abstract】 A new method for the determination of organophosphorus insecticide by solid phase microextraction (SPME) coupled with gas chromatography and mass spectrometric detection (GCMS) was developed. Some factors influencing SPME extraction efficiency such as ionic strength of solutions, absorption time and desorption time were studied. The extraction effects between two fiber coatings, polydimethylsiloxane (PDMS) and polyacrylate (PA), on organophosphorus insecticides were compared. The operating conditions of GCMS were also investigated. The results indicated that detection limits of parathion, methyl parathion, malathion and dichlorvos were in the range of 0004 μg/L to 040 μg/L, and the linearity correlation coefficients were 0998?4-0999?0. The recoveries of the four organophosphorus standards added in water were 947%-1101% with the relative standard deviations (RSD) from 162% to 825%. The proposed method has the advantages of solventfree sample preparation, simplicity of the procedure, good sensitivity and reproducibility.

【基金】 中国博士后科学基金资助项目(编号:2002032214);华中科技大学博士后科研基金专项基金.
  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2003年03期
  • 【分类号】O657.63
  • 【被引频次】88
  • 【下载频次】452
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