新型固相微萃取装置的研制及在有机磷农药检测中的应用  

A Study on New Solid Phase Micro-Extraction Device and Application of Organophosphorus Pesticides Determination

作　　者：顾涛[1] 帅琴[1] 高强[1] 肖红艳[2] 朱丹[1] 汤志勇[1] 

机构地区：[1]中国地质大学(武汉)材料与化学学院,湖北武汉430074 [2]地质过程与矿产资源国家重点实验室(中国地质大学),湖北武汉430074

出　　处：《岩矿测试》2012年第1期71-76,共6页Rock and Mineral Analysis

基　　金：国土资源地质大调查项目(1212011120274;1212011120281)

摘　　要：使用有机磷农药引起的环境污染问题日益严重,建立针对水体中有机磷农药的快速、灵敏、准确的检测方法,具有重要意义。文章采用溶胶-凝胶法自制一种有机-无机杂化涂层固相微萃取(SPME)探头,探头涂层呈多孔状。同时取用廉价易得的气相色谱进样针,设计了一种新的SPME装置。研究了SPME-GC/MS同时测定环境水样中甲拌磷、乙拌磷、甲基对硫磷、对硫磷、水胺硫磷5种有机磷农药的分析方法。方法检出限为1.2～3.9μg/L,相对标准偏差(RSD,n=6)为0.8%～7.4%。通过对实际样品的分析,方法加标回收率为93%～112%。建立的分析方法适合于环境水样中痕量有机磷农药的快速分析,具有一定的实用价值和应用前景。自制的有机-无机杂化涂层探头能重复使用达100余次,性能优于商用聚丙烯酸脂和聚二甲基硅氧烷涂层的萃取效果,通过更换探头,装置可重复使用。Currently, organophosphorus pesticides are widely used in agriculture, industry and other fields. However, they have also caused serious environmental pollution issues. Therefore, it is of valuable significance to establish a fast, sensitive and accurate detection method for organophosphorns pesticides in water. A Solid-Phase Micro-Extraction （SPME） probe with an organic/inoganic composite coating was prepared by a simple sol-gel method. A low-cost and convenient SPME device was developed by refitting a gas chromatogTaphy syringe. A new method has been established for simultaneous determination phorate, disulfoton, methyl parathion,parathion and isocarbophos in environmental water samples by SPME-Gas Chromatography （SPME-GC-MS）. The detection limits were between 1.2 μg/L and 3.9 μg/L. The relative standard deviations （RSD, n = 6） were between 0. 8% and 7.4%. The recoveries were between 93 and 112% for natural samples with an internal standard. The established method was qualified for fast determination of organophosphorns in environmental water sample with a good use value and potential. The organic/inorganic hybrid probe could be recycled up to 100 times, its extraction effect is better than that of commerical polyacrylate and polydimethylsiloxane （PDMS） probes. The SPME device could also be reused after probe replacement.

关 键 词：有机-无机杂化涂层 固相微萃取装置研制 有机磷农药 

分 类 号：O657.63[理学—分析化学] S482.33[理学—化学]