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采用邻菲啰啉铁纳米复合材料作为高效吸附剂,磁性分散固相萃取蜂蜜样品中的一些多环芳烃。

Magnetic dispersive solid-phase extraction of some polycyclic aromatic hydrocarbons from honey samples using iron (III) oxinate nanocomposite as an efficient sorbent.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.

Engineering Faculty, Near East University, Nicosia, Turkey.

出版信息

J Sep Sci. 2022 Jul;45(14):2642-2651. doi: 10.1002/jssc.202200212. Epub 2022 May 11.

Abstract

In this work, iron (III) oxinate magnetic nanocomposite was synthesized and employed as an efficient sorbent for the magnetic dispersive solid-phase extraction of some polycyclic aromatic hydrocarbons from honey samples. In the following, dispersive liquid-liquid microextraction procedure was used for further preconcentration of the analytes. The prepared sorbent was characterized using Fourier transform infrared spectrophotometry, X-ray diffractometry, vibrating sample magnetometry, energy dispersive X-ray spectroscopy, and scanning electron microscopy. The results verified the successful formation of the magnetic sorbent. In the extraction process, the sorbent was added into an aqueous solution and the mixture was vortexed. After completing the adsorption process, the supernatant phase was separated in the presence of a magnet and the analytes adsorbed onto sorbent were eluted by acetonitrile. Then, microliter-level 1,1,1-trichloroethane was mixed with the obtained acetonitrile and injected into NaCl solution. Finally, one microliter of the sedimented phase was injected into gas chromatography-flame ionization detector after centrifugation. Under the optimum conditions, a great repeatability (relative standard deviation equal or less than 5 and 6% for intra- and interday precisions, respectively), acceptable extraction recoveries (59-84%), high enrichment factors (118-168), and low limits of detection and quantification (0.16-0.36 and 0.56-1.22 ng/g, respectively) were acquired.

摘要

在这项工作中,合成了铁(III)邻苯二甲酸磁纳米复合材料,并将其用作从蜂蜜样品中提取一些多环芳烃的高效磁性分散固相萃取的吸附剂。接下来,采用分散液液微萃取法对分析物进行进一步预浓缩。使用傅里叶变换红外光谱法、X 射线衍射法、振动样品磁强计、能量色散 X 射线光谱法和扫描电子显微镜对制备的吸附剂进行了表征。结果验证了磁性吸附剂的成功形成。在萃取过程中,将吸附剂加入到水溶液中并进行涡旋混合。完成吸附过程后,在磁铁的存在下分离上清液,并用乙腈洗脱吸附在吸附剂上的分析物。然后,将微升级的 1,1,1-三氯乙烷与所得的乙腈混合,并注入到 NaCl 溶液中。最后,在离心后将沉淀相的 1 微升注入到气相色谱-火焰离子化检测器中。在最佳条件下,获得了很好的重复性(日内和日间精密度的相对标准偏差分别等于或小于 5%和 6%)、可接受的萃取回收率(59-84%)、高的富集因子(118-168)和低的检测限和定量限(分别为 0.16-0.36 和 0.56-1.22ng/g)。

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