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作 者:张凌怡[1] 张润生[2] 高方园[1,2] 张玉荣[2] 熊志超[1] 吴忠平[2] 张维冰[1]
机构地区:[1]上海市功能性材料化学重点实验室,华东理工大学,上海200237 [2]上海市公安局物证鉴定中心,上海市现场物证重点实验室-省部共建国家重点实验室培育基地,上海200083
出 处:《分析试验室》2014年第9期1024-1029,共6页Chinese Journal of Analysis Laboratory
基 金:上海市科学技术委员会科研计划项目(12JG0500200);公安部重点研究计划项目(201202ZDYJ005)资助
摘 要:将C18修饰的磁性纳米材料用于大体积水样中不同性质低浓度农药的分散固相萃取,并采用GC-MS进行检测。理论推导了样品添加回收率与磁性纳米颗粒密度、半径和用量之间的关系。当水样体积一定时,吸附材料用量越大,回收率越高,与实验结果一致。优化条件下,在0.1-10μg/L范围内线性相关系数大于0.9975(甲草胺除外,R^2=0.9684)。方法检出限(S/N=3)在0.006-0.05μg/L之间;回收率在13.4%-121.8%之间,标准偏差低于8.2%;最高富集倍数可达1484(氰戊菊酯)。方法可应用于大体积水样中低浓度非极性农药组分的检测。In this paper, octadecyl-functionalized magnetic nanoparticles (Fe3O4-C18 MNPs) were used as an adsorbent for analyzing trace pesticides in water samples coupled with gas chromatography-mass spectrometry. The theoretical relationships between recovery and the density, radius, amounts of magnetic nanoparticles were studied. The theory indicates that when the volume of solution was constant, the more the material used was, the higher the recovery was which was consistent with the experiment results. The optimized method shows good linearity with correlation coefficients over 0. 9975 in the concentration range of 0. 1 - 10 μ/L (except alachlor, R^2 =0. 9684), and affords low detection limits ( S/N = 3 ) from 0. 006 μg/L to 0. 05 μg/L. Average recoveries were in the range of 13. 4% - 121.8% with relative standard deviations below 8. 2%. A maximum enrichment factor of 1484 times was achieved for fenvalerate. Analysis results of poisoned pond water indicate that this method is fast, convenient, and efficient for the detection of low-concentration non-polar pesticides in aqueous samples.
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