School of Environmental & Municipal Engineering, State-Local Joint Engineering Research Center of Urban Sewage Treatment and Resource Recovery, Qingdao University of Technology, Qingdao 266033, China.
School of Environmental & Municipal Engineering, State-Local Joint Engineering Research Center of Urban Sewage Treatment and Resource Recovery, Qingdao University of Technology, Qingdao 266033, China.
J Chromatogr A. 2018 Jun 8;1553:57-66. doi: 10.1016/j.chroma.2018.04.034. Epub 2018 Apr 16.
A simple method of magnetic solid-phase extraction (MSPE) coupled to high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of four kinds of heterocyclic pesticides (carbendazim, triadimefon, chlorfenapyr and fenpyroximate) in environmental water samples. Magnetic metal-organic frameworks (MOFs) of type MOF-5 were prepared and used as adsorbents of MSPE. Several main parameters influencing MSPE efficiency were investigated, including amount of magnetic MOF-5, sample solution pH, extraction time, salt concentration, type and volume of desorption solvents and desorption time. Under optimal conditions, the MSPE-HPLC method presented fast simple separation and analysis, and excellent linearity in the range of 0.3-500.0 μg/L for carbendazim and triadimefon, and 0.1-500.0 μg/L for chlorfenapyr and fenpyroximate, with correlation coefficients (r) higher than 0.9992. High sensitivity with limits of detection and quantification ranging from 0.04-0.11 μg/L and 0.13-0.35 μg/L, respectively, were achieved, as well as good precision with relative standard deviations of 2.98-7.11% (intra-day) and 3.31-7.12% (inter-day). Furthermore, the method was successfully applied to reservoir and Yellow River water samples, and satisfactory recoveries at three spiked concentration levels were between 80.20% and 108.33%.The magnetic MOF-5 composites based MSPE followed by HPLC proved promising for convenient and efficient determination of heterocyclic pesticides in environmental water samples.
一种简单的磁固相萃取（MSPE）与高效液相色谱（HPLC）相结合的方法被开发出来，用于同时提取和测定环境水样中的四种杂环类农药（多菌灵、三唑酮、氯氟吡氧乙酸和氟吡甲禾灵）。采用磁性金属有机骨架（MOF）型 MOF-5 作为 MSPE 的吸附剂。考察了影响 MSPE 效率的几个主要参数，包括磁性 MOF-5 的用量、样品溶液 pH 值、萃取时间、盐浓度、解吸溶剂的种类和体积、解吸时间。在最佳条件下，MSPE-HPLC 方法具有快速简单的分离分析能力，在 0.3-500.0μg/L 范围内对多菌灵和三唑酮，以及 0.1-500.0μg/L 范围内对氯氟吡氧乙酸和氟吡甲禾灵均具有良好的线性关系，相关系数（r）均大于 0.9992。检测限和定量限分别为 0.04-0.11μg/L 和 0.13-0.35μg/L，灵敏度高，相对标准偏差（RSD）为 2.98-7.11%（日内）和 3.31-7.12%（日间），精密度良好。此外，该方法成功应用于水库和黄河水样，在三个加标浓度水平下的回收率在 80.20%-108.33%之间。基于磁性 MOF-5 复合材料的 MSPE 与 HPLC 相结合，为方便、高效地测定环境水样中的杂环类农药提供了一种有前景的方法。
