Ma Jiping, Hou Liwei, Wu Gege, Wang Liyan, Wang Xiaoyan, Chen Lingxin
School of Environmental & Municipal Engineering, Qingdao University of Technology, Qingdao 266033, China.
Key Laboratory of Coastal Environmental Processes and Ecological Remediation, Research Centre for Coastal Environmental Engineering and Technology, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China.
Materials (Basel). 2020 Dec 15;13(24):5729. doi: 10.3390/ma13245729.
Magnetic multi-walled carbon nanotubes were prepared as magnetic solid-phase extraction (MSPE) adsorbent for the enrichment of six heterocyclic pesticides in environmental water samples, including imidacloprid, triadimefon, fipronil, flusilazole, chlorfenapyr and fenpyroximate. Then six heterocyclic pesticides were separated and determined by high-performance liquid chromatography-diode-array detector (HPLC-DAD). Major factors influencing MSPE efficiency, including the dose of mag-multi-walled carbon nanotubes (mag-MWCNTs), extraction time, solution pH, salt concentration, type and volume of eluent and desorption time were investigated. Under the optimized conditions, the enrichment factor of the method reached to 250. The linearity was achieved within 0.05-10.0 μg/L for imidacloprid and chlorfenapyr, 0.10-10.0 μg/L for fipronil, flusilazole, triadimefon and fenpyroximate. Limits of detection were in the range of 0.01-0.03 μg/L. Good precision at three spiked levels were 1.1-11.2% (intra-day) and 1.7-11.0% (inter-day) with relative standard deviation of peak area, respectively. The developed method was utilized to analyze tap water, river water and reservoir water samples and recoveries at three spiked concentration levels ranged from 72.2% to 107.5%. The method was proved to be a convenient, rapid and practical method for sensitive determination of heterocyclic pesticides.
制备了磁性多壁碳纳米管作为磁性固相萃取（MSPE）吸附剂，用于富集环境水样中的六种杂环类农药，包括吡虫啉、三唑酮、氟虫腈、氟硅唑、氯虫苯甲酰胺和唑螨酯。然后，采用高效液相色谱 - 二极管阵列检测器（HPLC - DAD）对六种杂环类农药进行分离和测定。研究了影响MSPE效率的主要因素，包括磁性多壁碳纳米管（mag - MWCNTs）的用量、萃取时间、溶液pH值、盐浓度、洗脱剂的类型和体积以及解吸时间。在优化条件下，该方法的富集因子达到250。吡虫啉和氯虫苯甲酰胺在0.05 - 10.0 μg/L范围内、氟虫腈、氟硅唑、三唑酮和唑螨酯在0.10 - 10.0 μg/L范围内具有良好的线性关系。检测限在0.01 - 0.03 μg/L范围内。在三个加标水平下的精密度良好，峰面积的相对标准偏差分别为日内1.1 - 11.2%和日间1.7 - 11.0%。所建立的方法用于分析自来水、河水和水库水样，在三个加标浓度水平下的回收率为72.2%至107.5%。该方法被证明是一种方便、快速且实用的灵敏测定杂环类农药的方法。
