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超声辅助分散固相萃取法,使用负载在离子液体改性氧化石墨烯上的氮杂环卡宾铜配合物作为吸附剂,萃取三唑类杀菌剂。

Ultrasound assisted dispersive solid phase extraction of triazole fungicides by using an N-heterocyclic carbene copper complex supported on ionic liquid-modified graphene oxide as a sorbent.

机构信息

Faculty of Chemistry, Shahid Beheshti University, G. C., P.O. Box 1983963113, Evin, Tehran, Iran.

出版信息

Mikrochim Acta. 2019 Mar 2;186(4):209. doi: 10.1007/s00604-019-3276-1.

DOI:10.1007/s00604-019-3276-1
PMID:30826862
Abstract

An ultrasound-assisted method is described for dispersive solid phase extraction of trace levels of triazole fungicides. A sorbent was prepared from an N-heterocyclic carbene copper complex that was supported on ionic liquid-modified graphene oxide. The sorbent was characterized by scanning electron microscopy, transmission electron microscopy, Raman and FT-IR spectroscopy, energy-dispersive X-ray spectroscopy and elemental mapping. The capability of sorption and extraction is mainly based on complexation with Cu (I) ions. The variables affecting extraction were optimized. Following desorption with ethanol, the fungicides were quantified by corona discharge ion mobility spectrometry. Under optimized conditions (solution pH value: 7.0; amount of sorbent: 10 mg; extraction time: 3 min; desorption agent: ethanol), the technique provides good linearity (>0.994), repeatability (RSD < 4.1%), low limits of detection (0.18 ng.mL), excellent preconcentration factors (468-476) and high recoveries from spiked environmental water samples (92-94%). The sorbent can be reused over five cycles without significant loss of its activity. Graphical abstract Schematic presentation of design and synthesis of the N-heterocyclic carbene copper complex supported on ionic liquid-modified graphene oxide as a sorbent for triazole fungicides and its application in ultrasound-assisted dispersive solid phase extraction with ion mobility spectrometric detection.

摘要

超声辅助分散固相萃取痕量三唑类杀菌剂的方法。将 N-杂环卡宾铜配合物负载在离子液体改性氧化石墨烯上制备了一种吸附剂。采用扫描电子显微镜、透射电子显微镜、拉曼和 FT-IR 光谱、能量色散 X 射线光谱和元素映射对吸附剂进行了表征。吸附和萃取的能力主要基于与 Cu(I)离子的络合。优化了影响萃取的变量。用乙醇解吸后,用电晕放电离子迁移谱法定量测定了杀菌剂。在优化条件下(溶液 pH 值:7.0;吸附剂用量:10 mg;萃取时间:3 min;解吸剂:乙醇),该技术具有良好的线性(>0.994)、重复性(RSD<4.1%)、低检测限(0.18 ng.mL)、高浓缩因子(468-476)和从加标环境水样中获得的高回收率(92-94%)。吸附剂可重复使用五次以上,而其活性无明显损失。

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星形聚噻吩树枝状大分子涂层用于三唑类农药的固相微萃取。
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