Department of Applied Chemistry, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
Department of Applied Chemistry, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
Talanta. 2017 May 1;166:93-100. doi: 10.1016/j.talanta.2017.01.051. Epub 2017 Jan 17.
In this research, a novel method using magnetic mixed hemimicelles dispersive solid-phase extraction (MMHDSPE) based on CmimBr-coated attapulgite/polyaniline-polypyrrole/FeO (ATP/PANI-PPY/FeO) nanocomposites were investigated for enrichment and separation of three acaricides in fruit juice. In this method, we combined the simplicity and speed of dispersive solid-phase extraction, the advantages of mixed hemimicelles and the facility of the phase separation of the magnetic nanoparticles to develop a simple, rapid, sensitive, and effective method for detecting target analytes from the juice samples. ATP/PANI-PPY/FeO nanocomposites were successfully synthesized using a one-pot method. The as-prepared nanocomposite sorbents were characterized by Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The experimental factors affecting the extraction efficiency including the sorbent type, amount of ATP/PANI-PPY/FeO nanocomposites, volume of ILs, sonication time, pH, and desorption conditions were optimized. Under the optimal conditions, good linearity was observed for all target analytes, with correlation coefficients (r) ranging from 0.9994 to 0.9999; the limits of detection (LOD) were in the range of 0.16-0.57μgL, and the recoveries of analytes using the proposed method ranged between 88.67% and 95.10%. The sorbents exhibited excellent repeatability in the range of 1.83-4.24% in extracting the three target analytes. In addition, the intra-day and inter-day precision values were found to be in the range of 0.19-6.24% and 2.23-8.36%, respectively. The method was successfully applied to analyze fruit juice samples by rapid preconcentration of acaricides.
在这项研究中,我们研究了一种基于 CmimBr 包覆的凹凸棒土/聚苯胺-聚吡咯/FeO(ATP/PANI-PPY/FeO)纳米复合材料的新型磁性混合半胶束分散固相萃取(MMHDSPE)方法,用于果汁中三种杀螨剂的富集和分离。在这种方法中,我们结合了分散固相萃取的简单性和速度、混合半胶束的优点以及磁性纳米粒子相分离的便利性,开发了一种从果汁样品中检测目标分析物的简单、快速、灵敏、有效的方法。采用一锅法成功合成了 ATP/PANI-PPY/FeO 纳米复合材料。采用傅里叶变换红外光谱(FT-IR)、X 射线衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对所制备的纳米复合材料进行了表征。优化了影响萃取效率的实验因素,包括吸附剂类型、ATP/PANI-PPY/FeO 纳米复合材料用量、IL 体积、超声时间、pH 值和洗脱条件。在最佳条件下,所有目标分析物均表现出良好的线性关系,相关系数(r)范围为 0.9994-0.9999;检测限(LOD)范围为 0.16-0.57μg/L,采用所提出的方法,分析物的回收率在 88.67%-95.10%之间。该吸附剂在 1.83-4.24%范围内对三种目标分析物的提取具有良好的重复性。此外,日内和日间精密度值分别在 0.19%-6.24%和 2.23%-8.36%范围内。该方法成功应用于快速预浓缩杀螨剂分析果汁样品。