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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
【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 (GCMS) 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 GCMS were also investigated. The results indicated that detection limits of parathion, methyl parathion, malathion and dichlorvos were in the range of 0004 μg/L to 040 μg/L, and the linearity correlation coefficients were 0998?4-0999?0. The recoveries of the four organophosphorus standards added in water were 947%-1101% with the relative standard deviations (RSD) from 162% to 825%. The proposed method has the advantages of solventfree sample preparation, simplicity of the procedure, good sensitivity and reproducibility.
【Key words】 solid phase microextraction; gas chromatography; mass spectrometry; organophosphorus insecticide; water analysis;
- 【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