基于石墨烯泡沫的电增强固相微萃取-高效液相色谱法测定鱼肉中3 种磺胺类的残留

doi:10.7506/spkx1002-6630-20230822-160

食品科学 ›› 2024, Vol. 45 ›› Issue (5): 265-274.doi: 10.7506/spkx1002-6630-20230822-160

基于石墨烯泡沫的电增强固相微萃取-高效液相色谱法测定鱼肉中3 种磺胺类的残留

孙瑞雪，方禹文，陈冬妍，陈全胜，陈晓梅

（集美大学海洋食品与生物工程学院，福建厦门 361021）

出版日期:2024-03-15 发布日期:2024-04-03
基金资助:
国家自然科学基金面上项目（32072299）

Determination of the Residues of Three Sulfonamides in Fish by Graphene Foam-Based Electro-Enhanced Solid-Phase Microextraction Coupled with High Performance Liquid Chromatography

SUN Ruixue, FANG Yuwen, CHEN Dongyan, CHEN Quansheng, CHEN Xiaomei

(College of Ocean Food and Biological Engineering, Jimei University, Xiamen 361021, China)

Online:2024-03-15 Published:2024-04-03

摘要/Abstract

摘要： 为提高鱼肉中磺胺类抗生素（sulfonamides，SAs）残留的富集效果，建立了基于氮掺杂三维石墨烯泡沫功能化整体柱（monolith@nitrogen-doped three-dimensional graphene foam，M@NGF）的电增强固相微萃取（electro-enhanced solid phase microextraction，EE-SPME）方法，结合高效液相色谱技术，快速、灵敏地测定鱼肉中SAs残留。本研究采用原位聚合法，以离子液体为功能单体，NGF为导电增强剂，在不锈钢丝表面制备多孔M@NGF，建立EE-SPME方法，从鱼肉中萃取磺胺噻唑（sulfathiazole，ST）、磺胺二甲基嘧啶（sulfamethazine，SM2）和磺胺二甲氧嘧啶（sulfadimethoxypyrimidine，SMM）。对吸附时间、搅拌速度、吸附电压、离子强度、样品溶液pH值、解吸时间、解吸电压和解吸液组成进行了优化。结果表明，基于M@NGF的EE-SPME法对ST、SM2和SMM的富集倍数分别为74、58和64，吸附平衡时间缩短至35 min。在5～5 000 μg/kg线性范围内，本方法对ST、SM2和SMM的检出限分别为1.78、3.16 μg/kg和1.84 μg/kg，定量限均为5 μg/kg，线性回归分析的决定系数（R2）均大于0.999 0，加标回收率为79.2%～110.1%，相对标准偏差范围为1.4%～9.8%（n＝5）。本方法解决了鱼肉中SAs残留萃取效率低、基质干扰严重的问题，实现了鱼肉中SAs残留的快速、灵敏检测。

关键词: 石墨烯泡沫；电增强固相微萃取；高效液相色谱法；磺胺类残留；鱼肉

Abstract: A rapid and sensitive method for the determination of sulfonamide (SA) residues in fish was developed using electro-enhanced solid-phase microextraction (EE-SPME) based on nitrogen-doped three-dimensional graphene foam (NGF) functionalized monolithic column (monolith@NGF, M@NGF) combined with high performance liquid chromatography (HPLC). To improve the enrichment efficiency of SA residues in fish, porous M@NGF was prepared on the surface of stainless-steel wires by in situ polymerization using ionic liquids as the functional monomer and NGF as the conductivity enhancer. The EE-SPME method was applied for the extraction of sulfathiazole (ST), sulfamethazine (SM2), and sulfadimethoxypyrimidine (SMM) from fish. Adsorption time, agitation speed, adsorption voltage, ionic strength, the pH of sample solution, desorption time, desorption voltage, and the composition of desorption solution were optimized. The results showed that the M@NGF-based EE-SPME method enriched ST, SM2 and SMM by 74, 58 and 64 folds, respectively, and shortened the adsorption equilibrium time to 35 min. In the linear range of 5–5 000 μg/kg, the limits of detection (LODs) of this method were 1.78, 3.16 and 1.84 μg/kg for ST, SM2 and SMM, respectively, and the limits of quantification (LOQs) were 5 μg/kg for all analytes. Coefficients of determination (R2) for linear regression analysis of this method were all greater than 0.999 0, and the recoveries from spiked samples ranged from 79.2% to 110.1%, with relative standard deviations (RSDs) ranging from 1.4% to 9.8% (n = 5). This method solved the problems of low extraction efficiency and serious matrix interference of SA residues in fish, and allowed the rapid, sensitive detection of SA residues in fish.

Key words: graphene foam; electro-enhanced solid-phase microextraction; high performance liquid chromatography; sulfonamide residues; fish

中图分类号:

TS254.7

孙瑞雪，方禹文，陈冬妍，陈全胜，陈晓梅. 基于石墨烯泡沫的电增强固相微萃取-高效液相色谱法测定鱼肉中3 种磺胺类的残留[J]. 食品科学, 2024, 45(5): 265-274.

SUN Ruixue, FANG Yuwen, CHEN Dongyan, CHEN Quansheng, CHEN Xiaomei. Determination of the Residues of Three Sulfonamides in Fish by Graphene Foam-Based Electro-Enhanced Solid-Phase Microextraction Coupled with High Performance Liquid Chromatography[J]. FOOD SCIENCE, 2024, 45(5): 265-274.

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基于石墨烯泡沫的电增强固相微萃取-高效液相色谱法测定鱼肉中3 种磺胺类的残留

Determination of the Residues of Three Sulfonamides in Fish by Graphene Foam-Based Electro-Enhanced Solid-Phase Microextraction Coupled with High Performance Liquid Chromatography

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