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采用超高效液相色谱-串联质谱法,通过选择性磁固相萃取从鱼类样品中提取酰胺类除草剂。

Selective magnetic solid-phase extraction of amide herbicides from fish samples coupled with ultra-high-performance liquid chromatography with tandem mass spectrometry.

机构信息

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.

出版信息

J Sep Sci. 2022 Feb;45(4):896-907. doi: 10.1002/jssc.202100823. Epub 2021 Dec 16.

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.

摘要

一种高效的磁性假模板分子印迹聚合物纳米复合材料,使用多壁碳纳米管作为载体,以灭草隆去氯作为假模板进行制备。采用傅里叶变换红外光谱、振动样品磁强计、扫描电子显微镜和透射电子显微镜对所得到的纳米复合材料进行了表征。通过结合实验,包括静态吸附、动力学吸附和选择性识别研究,评估了所得到的纳米复合材料的吸附性能。将所得到的纳米复合材料成功地应用于从鱼样中通过液相色谱-串联质谱法进行的七种酰胺类除草剂(甲草胺、乙草胺、异丙甲草胺、丁草胺、灭草隆、乙草胺乙酯和二甲戊乐灵)的磁性固相萃取作为选择性吸附剂。在优化条件下,酰胺类除草剂的检出限为 0.01-0.1μg/kg。从鱼样中获得的酰胺类除草剂的回收率在 88.0%至 102.1%之间,相对标准偏差小于 7.5%。与文献报道的方法相比,这种方法消除了模板泄漏对定性和定量分析的影响,被证明优于文献方法。结果表明,它可以成功地应用于分析鱼样中的酰胺类除草剂,具有令人满意的回收率。

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