分散液相微萃取-气相色谱联用分析水样中菊酯类农药残留  

Analysis of Pyrethroid Pesticides in Water Samples by Dispersive Liquid-liquid Microextraction Coupled with Gas Chromatography

作　　者：臧晓欢[1] 王春[1] 高书涛[1] 周欣[1] 王志[1] 

机构地区：[1]河北农业大学理学院,生物无机化学重点实验室,保定071001

出　　处：《分析化学》2008年第6期765-769,共5页Chinese Journal of Analytical Chemistry

基　　金：河北省自然科学基金资助项目(NO.B2006000413);河北农业大学科研发展基金资助项目

摘　　要：将分散液-液微萃取(DLLME)与气相色谱-电子俘获检测(GC-ECD)技术相结合,建立了高灵敏度测定水样中7种菊酯类农药残留的新方法。对影响萃取富集效率的因素进行优化,萃取条件选定为:在5.0mL样品溶液中加入10.0μL氯苯和1.0mL丙酮,分散混匀后,以5000r/min离心5min,吸出萃取溶剂氯苯直接进样分析。在优化条件下7种菊酯类农药的富集倍数高达708～1087倍。以α-六六六为内标,7种菊酯类农药在0.8～600μg/L范围内具有良好的线性关系,线性相关系数在0.9990～0.9999之间;检出限为0.04～0.10μg/L(S/N=3)。本方法已应用于自来水、井水及河水等实际水样的分析,平均加标回收率在76.0%～116.0%之间;相对标准偏差在3.1%～7.2%之间。方法具有操作简单、富集效率高和灵敏度高等特点,可满足水样中菊酯类农药残留的检测要求。A novel method was developed for the determination of pyrethroid pesticide residues in water sampies by dispersive liquid-liquid microextraction （DLLME）coupled with capillary gas chromatography with electron capture detection（GC-ECD）. Some important parameters that influence the extraction efficiency, such as the kind of the extraction and disperser solvent, their volume the method, 10.0 μL chlorobenzene and 1.0 mL acetone were After centrifugation at 5000 r/min for 5 min, the sedimented and the extraction time, were investigated. In rapidly injected into a 5.0- mL water sample. chlorobenzene phase was directly injected into the GC for analysis. Under the optimum conditions, as high as 708-to 1087-fold enrichment factors were achieved. Using a-benzene hexachloride as the internal standard, a good linear relationship was obtained in the range of 0.8 -600 μg/L of the analytes with the correlation coefficients of 0.9990 -0.9999 and the detection limits of 0.04 -0.10μg/L （S/N = 3 ）, respectively. This method has been successfully applied for the determination of pyrethroid pesticide residues in real water samples（ tap, well and river waters） with satisfactory results. The recoveries fell in the range from 76.0% to 116.0% and the relative standard deviations were between 3, 1% and 7.2%. The method was proven to be simple and environmental benign with high enrichment factor and low cost.

关 键 词：分散液相微萃取 气相色谱 菊酯类农药 水样 

分 类 号：X832[环境科学与工程—环境工程] O661.1[理学—分析化学]