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Selective magnetic solid-phase extraction of amide herbicides from fish samples coupled with ultra-high-performance liquid chromatography with tandem mass spectrometry
Authors:Lei Gao  Dongli Qin  Zhongxiang Chen  Shuyan Bai  Ningning Du  Chenhui Li  Qirui Hao  Peng Wang
Institution:1. Heilongjiang River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Harbin, P. R. China;2. Heilongjiang River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Harbin, P. R. China

Supervision, Inspection and Testing Center for Fishery Environment and Aquatic Products (Harbin), Ministry of Agriculture and Rural Affairs, Harbin, P. R. China

Laboratory of Quality and Safety Risk Assessment for Aquatic Products (Harbin), Ministry of Agriculture and Rural Affairs, Harbin, P. R. China

Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture and Rural Affairs, Beijing, P. R. China;3. Heilongjiang River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Harbin, P. R. China

Supervision, Inspection and Testing Center for Fishery Environment and Aquatic Products (Harbin), Ministry of Agriculture and Rural Affairs, Harbin, P. R. China

Laboratory of Quality and Safety Risk Assessment for Aquatic Products (Harbin), Ministry of Agriculture and Rural Affairs, Harbin, P. R. China

Abstract:An efficient magnetic dummy template molecularly imprinted polymer nanocomposite was prepared using multi-walled carbon nanotubes as a support and metolachlor deschloro as a dummy template. The obtained nanocomposites were characterized using Fourier transform infrared spectroscopy, vibrating sample magnetometry, scanning electron microscopy, and transmission electron microscopy. The adsorption performance of the obtained nanocomposites was evaluated through binding experiments, including static adsorption, kinetic adsorption, and selective recognition studies. The obtained nanocomposites were successfully applied as selective sorbents for the magnetic solid-phase extraction of seven amide herbicides (alachlor, acetochlor, pretilachlor, butachlor, metolachlor, diethatyl ethyl, and dimethachlor) coupled with liquid chromatography-tandem mass spectrometry from fish samples. Under the optimized conditions, the limit of detection was 0.01–0.1 μg/kg. The obtained recoveries of the amide herbicides from the fish samples were in the range of 88.0 to 102.1% with a relative standard deviation of less than 7.5%. This method, which eliminated the effect of template leakage on qualitative and quantitative analysis was found to be superior to the methods reported in the literature. The results indicated that it could be successfully applied to analyze amide herbicides in fish samples with satisfactory recoveries.
Keywords:amide herbicides  fish samples  magnetic solid-phase extraction  selective extraction
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