适配体功能化磁性纳米/氧化石墨烯固相萃取-超高效液相色谱法测定玉米赤霉烯酮

doi:10.7506/spkx1002-6630-20260206-058

食品科学 ›› 2026, Vol. 47 ›› Issue (15): 317-326.doi: 10.7506/spkx1002-6630-20260206-058

适配体功能化磁性纳米/氧化石墨烯固相萃取-超高效液相色谱法测定玉米赤霉烯酮

罗丽红，劳水兵，牙禹，李慧玲，韦宇宁，何洁，梁志俭，黄芳，周其峰，覃国新

（广西壮族自治区农业科学院农产品质量安全与检测技术研究所，广西?南宁 530007）

出版日期:2026-08-15 发布日期:2026-08-24
基金资助:
广西自然科学基金项目（2023GXNSFAA026442；2025GXNSFAA069262）；广西农业科学院基本科研业务专项（2025YP107；2026YT153；2026YT154）；科技先锋队“强农富民”“六个一”专项行动项目（桂农科盟202416）

Determination of Zearalenone by Ultra-high Performance Liquid Chromatography Coupled with Solid-Phase Extraction Using Aptamer-Functionalized Magnetic Fe3O4 Nanoparticles/Graphene Oxide as Sorbent

LUO Lihong, LAO Shuibing, YA Yu, LI Huiling, WEI Yuning, HE Jie, LIANG Zhijian, HUANG Fang, ZHOU Qifeng, QIN Guoxin

(Agro-Products Quality Safety and Testing Technology Research Institute, Guangxi Academy of Agricultural Sciences, Nanning 530007, China)

Online:2026-08-15 Published:2026-08-24

摘要/Abstract

摘要： 通过化学共沉淀法合成适配体功能化的磁性氧化石墨烯纳米颗粒（aptamer-functionalized Fe3O4/graphene oxide，Apt/Fe3O4/GO），并将其作为磁固相萃取中的吸附剂。采用傅里叶变换红外光谱、透射电子显微镜、X射线衍射、振动样品磁强计和X射线光电子能谱等多种技术对制备的材料进行表征，以证明Apt/Fe3O4/GO的成功制备。建立超高效液相色谱-荧光检测（ultra-high performance liquid chromatography-fluorescence detection，UPLC-FLD）与Apt/Fe3O4/GO磁固相萃取（magnetic solid-phase extraction，MSPE）相结合的方法并优化萃取参数，用于检测玉米和小麦样品中的玉米赤霉烯酮。结果表明，在优化条件下，分析物可在11 min内完成前处理工作。所建立的MSPE-UPLC-FLD方法在8.0～1 000.0 ng/mL的质量浓度范围内表现出良好的线性关系，检测限为2.64 ng/mL，实际样品回收率为88.2%～101.8%。经过8 次重复使用后，回收率仍保持在80.5%左右。本研究制备的Apt/Fe3O4/GO结合适配体和Fe3O4/GO的磁性优势，可显著提高玉米赤霉烯酮的检测效率、灵敏度和选择性，在食品分析中具有良好的应用价值。

关键词: 适配体；Fe3O4；氧化石墨烯；玉米赤霉烯酮；超高效液相色谱；磁固相萃取

Abstract: Aptamer-functionalized Fe3O4 nanoparticles/graphene oxide (Apt/Fe3O4/GO) was synthesized by the chemical co-precipitation method for use as a sorbent for magnetic solid-phase extraction (MSPE). The prepared material was characterized using various techniques such as Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and X-ray photoelectron spectroscopy (XPS) to demonstrate the successful preparation of Apt/Fe3O4/GO. Subsequently, an ultra-high performance liquid chromatography with fluorescence detection (UPLC-FLD) method was established for the detection of zearalenone (ZEN) in corn and wheat samples after MSPE using Apt/Fe3O4/GO. Important operating parameters including sample pH, extraction time, and desorption conditions were optimized. The results indicated that under optimized conditions, the pretreatment procedure was achieved within 11 minutes. The established MSPE-UPLC-FLD method showed a good linear relationship in the concentration range of 8.0–1 000.0 ng/mL, with a detection limit (LOD) of 2.64 ng/mL. The recoveries for actual samples ranged from 88.2% to 101.8%. After 8th repeated use, the recovery remained at around 80.5%. In conclusion, Apt/Fe3O4/GO combines the magnetic advantages of Fe3O4/GO and the recognition ability of aptamers, significantly improving the detection efficiency, sensitivity, and selectivity of ZEN. This composite holds great application value in food analysis.

Key words: aptamer; Fe3O4; graphene oxide; zearalenone; ultra-high performance liquid chromatography; magnetic solid phase extraction

中图分类号:

TS207.3

罗丽红，劳水兵，牙禹，李慧玲，韦宇宁，何洁，梁志俭，黄芳，周其峰，覃国新. 适配体功能化磁性纳米/氧化石墨烯固相萃取-超高效液相色谱法测定玉米赤霉烯酮[J]. 食品科学, 2026, 47(15): 317-326 https://doi.org/10.7506/spkx1002-6630-20260206-058

LUO Lihong, LAO Shuibing, YA Yu, LI Huiling, WEI Yuning, HE Jie, LIANG Zhijian, HUANG Fang, ZHOU Qifeng, QIN Guoxin. Determination of Zearalenone by Ultra-high Performance Liquid Chromatography Coupled with Solid-Phase Extraction Using Aptamer-Functionalized Magnetic Fe3O4 Nanoparticles/Graphene Oxide as Sorbent[J]. FOOD SCIENCE, 2026, 47(15): 317-326 https://doi.org/10.7506/spkx1002-6630-20260206-058

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适配体功能化磁性纳米/氧化石墨烯固相萃取-超高效液相色谱法测定玉米赤霉烯酮

Determination of Zearalenone by Ultra-high Performance Liquid Chromatography Coupled with Solid-Phase Extraction Using Aptamer-Functionalized Magnetic Fe3O4 Nanoparticles/Graphene Oxide as Sorbent

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