Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Synthesis and Application of Organic Functional Molecules, College of Chemistry and Chemical Engineering, Hubei University, Wuhan, P. R. China.
J Sep Sci. 2020 Apr;43(8):1514-1522. doi: 10.1002/jssc.201900896. Epub 2020 Apr 2.
In this study, porous sandwich structure Fe O nanoparticles coated by polyhedral oligomeric silsesquioxanes and β-cyclodextrin were prepared by surface polymerization and were used as the magnetic solid phase extraction adsorbent for the extraction and determination of carbaryl and carbofuran. The Fe O nanoparticles coated with polyhedral oligomeric silsesquioxanes and β-cyclodextrin were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, thermogravimetric analysis, vibrating sample magnetometry, and scanning electron microscopy. After optimizing the extraction conditions, a method that combined magnetic solid phase extraction with high-performance liquid chromatography was developed for the determination of carbaryl and carbofuran in apple. The method exhibited a good linearity in the range of 2-400 μg/kg for carbaryl and carbofuran (R = 0.9995), respectively. The limits of detection were 0.5 μg/kg of carbaryl and 0.7 μg/kg for carbofuran in apple, respectively. Extraction recoveries ranged from 94.2 to 103.1% with the preconcentration factor of 300 and the relative standard deviations were less than 5.9%. These results indicated that the method combined magnetic solid phase extraction with high-performance liquid chromatography and was promising for the determination of carbaryl and carbofuran at trace amounts.
在这项研究中，通过表面聚合制备了多面体低聚倍半硅氧烷和β-环糊精包覆的多孔夹层结构 Fe3O4纳米粒子，并将其用作磁性固相萃取吸附剂，用于提取和测定克百威和呋喃丹。通过傅里叶变换红外光谱、X 射线衍射、热重分析、振动样品磁强计和扫描电子显微镜对多面体低聚倍半硅氧烷和β-环糊精包覆的 Fe3O4纳米粒子进行了表征。在优化了萃取条件后，建立了一种结合磁性固相萃取和高效液相色谱法测定苹果中克百威和呋喃丹的方法。该方法对克百威和呋喃丹的线性范围分别为 2-400μg/kg（R=0.9995）。克百威和呋喃丹在苹果中的检出限分别为 0.5μg/kg 和 0.7μg/kg。在预浓缩因子为 300 的情况下，提取回收率在 94.2%至 103.1%之间，相对标准偏差小于 5.9%。这些结果表明，该方法结合了磁性固相萃取和高效液相色谱法，有望用于痕量克百威和呋喃丹的测定。
