Department of Analytical Chemistry, Faculty of Chemistry, University of Mazandaran, Babolsar, Iran.
J Sep Sci. 2018 May;41(9):2037-2045. doi: 10.1002/jssc.201701090. Epub 2018 Feb 27.
Sodium dodecyl sulfate coated amino-functionalized magnetic iron oxide nanoparticles were used as an efficient adsorbent for rapid removal and preconcentration of three important organophosphorus pesticides, chlorpyrifos, diazinon and phosalone, by ultrasound-assisted dispersive magnetic solid-phase microextraction. Fabrication of amino-functionalized magnetic nanoparticles was certified by characteristic analyses, including Fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, and transmission electron microscopy. Affecting parameters on the removal efficiency were investigated and optimized through half-fractional factorial design and Doehlert design, respectively. The analysis of analytes was performed by high-performance liquid chromatography with ultraviolet detection. Under the optimum conditions, extraction recoveries for 20 ng/mL of organophosphorus pesticides were in the range of 84-97% with preconcentration factors in the range of 134-155. Replicating the experiment in above condition for five times gave the relative standard deviations <6%. The calibration curves showed high linearity in the range of 0.2-700 ng/mL and the limits of detection were in the range of 0.08-0.13 ng/mL. The proposed method was successfully applied for both removal and trace determination of these three organophosphorus pesticides in environmental water and fruit juice samples.
十二烷基硫酸钠包覆的氨基功能化磁性氧化铁纳米粒子被用作一种高效的吸附剂,通过超声辅助分散磁性固相微萃取快速去除和预浓缩三种重要的有机磷农药,氯吡硫磷、二嗪农和磷丹。氨基功能化磁性纳米粒子的制备通过特征分析得到了证实,包括傅里叶变换红外光谱、热重分析、扫描电子显微镜和透射电子显微镜。通过半析因设计和 Doehlert 设计分别考察和优化了影响去除效率的参数。通过高效液相色谱法与紫外检测对分析物进行分析。在最佳条件下,20ng/mL 有机磷农药的萃取回收率在 84-97%之间,浓缩因子在 134-155 之间。在上述条件下重复实验五次,相对标准偏差<6%。校准曲线在 0.2-700ng/mL 范围内具有高线性,检出限在 0.08-0.13ng/mL 范围内。该方法成功应用于环境水样和果汁样品中这三种有机磷农药的去除和痕量测定。