Wang Shuo, Zhao Peng, Min Guang, Fang Guozhen
Tianjin Key Laboratory of Food Nutrition and Safety, Faculty of Food Engineering and Biotechnology, Tianjin University of Science and Technology, Tianjin 300457, China.
J Chromatogr A. 2007 Sep 21;1165(1-2):166-71. doi: 10.1016/j.chroma.2007.07.061. Epub 2007 Aug 1.
A reliable multi-residue method which was based on solid-phase extraction (SPE) with multi-walled carbon nanotubes (MWCNTs) as adsorbent was developed for determination and quantitation of 12 pesticides (carbofuran, iprobenfos, parathion-methyl, prometryn, fenitrothion, parathion-ethyl, isocarbofos, phenthoate, methidathion, endrin, ethion, methoxychlor) in surface water by gas chromatography-mass spectrometry (GC-MS). Parameters that might influence the extraction efficiency such as the eluent volume, the sample flow rate and the sample loading volume were optimized. The experimental results showed the excellent linearity of 12 pesticides (R(2)>0.99) over the range of 0.04-4 microg L(-1), and the precisions (RSD) were 3.1-15.1% under the optimal conditions. The detection limits of proposed method could reach 0.01-0.03 microg L(-1) based on the ratio of chromatographic signal to base line noise (S/N=3). Good recoveries achieved with spiked water samples were in the range of 82.0-103.7%. The results indicated that MWCNTs have good adsorbability to the 12 pesticides tested in this study. With less cost, less analytical time and less solvent-consuming, the developed multi-residue method could be used to determine multi-class pesticides in water simultaneously.
建立了一种基于多壁碳纳米管（MWCNTs）作为吸附剂的固相萃取（SPE）的可靠多残留方法，用于通过气相色谱-质谱联用（GC-MS）测定和定量地表水中的12种农药（克百威、异稻瘟净、甲基对硫磷、扑草净、杀螟硫磷、对硫磷、水胺硫磷、稻丰散、杀扑磷、异狄氏剂、乙硫磷、甲氧滴滴涕）。优化了可能影响萃取效率的参数，如洗脱液体积、样品流速和进样体积。实验结果表明，12种农药在0.04-4μg L(-1)范围内具有良好的线性（R(2)>0.99），在最佳条件下精密度（RSD）为3.1-15.1%。基于色谱信号与基线噪声之比（S/N=3），该方法的检测限可达0.01-0.03μg L(-1)。加标水样的回收率在82.0-103.7%范围内。结果表明，MWCNTs对本研究中测试的12种农药具有良好的吸附性。该多残留方法成本低、分析时间短、溶剂消耗少，可用于同时测定水中的多类农药。
