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发展水相兼容的分子印迹固相萃取技术,并结合高效液相色谱-串联质谱法,用于检测动物源性食品中的六种磺胺类药物。

Development of water-compatible molecularly imprinted solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry for the detection of six sulfonamides in animal-derived foods.

机构信息

Key Laboratory of Food Nutrition and Safety, Ministry of Education, Tianjin University of Science & Technology, 29 The Thirteenth Road, Tianjin Economy and Technology Development Area, Tianjin, 300457, PR China.

Biotechnology Research Institute, Chinese Academy of Agricultural Sciences, Haidian District, Beijing, 010010, PR China.

出版信息

J Chromatogr A. 2018 Nov 2;1574:9-17. doi: 10.1016/j.chroma.2018.08.044. Epub 2018 Aug 22.

Abstract

A water-compatible molecularly imprinted polymer (MIP) was prepared by combining reversible addition-fragmentation chain transfer (RAFT) with reflux precipitation polymerization (RPP) for solid-phase extraction (SPE) coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) to detect six sulfonamides (SAs) in animal-derived foods and water samples. The SEM images indicated the spherical structure of MIP materials. In water medium, MIPs still performed good specific adsorption for SAs. Under the optimized detection conditions, the proposed method offered good linearity (R > 0.996) for the six SAs with relative standard deviation (RSD) for ten replicate extractions of 1.64%-4.68%, limits of detection (S/N = 3) of 0.02 μg L-0.1 μg L and recoveries of 63.49%-115.72%. Besides, the whole extract process avoided organic solvent consumption, and trace sulfadiazine residues were found in the pork sample at similar concentration of 3.57 and 3.79 μg kg using the MIP-SPE method and commercial Oasis HLB cartridge, respectively. It is confirmed the method could be applied to quantitative detect the trace residue sulfonamides in animal-derived samples and water samples.

摘要

一种水相兼容的分子印迹聚合物(MIP)通过可逆加成-断裂链转移(RAFT)与回流沉淀聚合(RPP)相结合制备,用于固相萃取(SPE)与高效液相色谱-串联质谱(HPLC-MS/MS)联用,检测动物源性食品和水样中的六种磺胺类药物(SAs)。SEM 图像表明 MIP 材料具有球形结构。在水介质中,MIP 对 SAs 仍表现出良好的特异性吸附。在优化的检测条件下,该方法对六种磺胺类药物具有良好的线性(R>0.996),十个重复提取的相对标准偏差(RSD)为 1.64%-4.68%,检测限(S/N=3)为 0.02μg L-0.1μg L,回收率为 63.49%-115.72%。此外,整个提取过程避免了有机溶剂的消耗,使用 MIP-SPE 方法和商业 Oasis HLB 萃取小柱在浓度相似的情况下(分别为 3.57μgkg 和 3.79μgkg)在猪肉样品中均检测到痕量磺胺嘧啶残留。证实该方法可用于定量检测动物源性样品和水样中的痕量残留磺胺类药物。

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