食品科学2025,Vol.46Issue(3) :222-229.DOI:10.7506/spkx1002-6630-20240718-183

金属有机骨架基固相萃取-高效液相色谱法检测水产品中5种氟喹诺酮类药物残留

Determination of Five Fluoroquinolones in Aquatic Products by High Performance Liquid Chromatography with Solid Phase Extraction Using Metal-Organic Framework as Sorbent

牛灿杰 叶素丹 朱千聪 胡玉霞
食品科学2025,Vol.46Issue(3) :222-229.DOI:10.7506/spkx1002-6630-20240718-183

金属有机骨架基固相萃取-高效液相色谱法检测水产品中5种氟喹诺酮类药物残留

Determination of Five Fluoroquinolones in Aquatic Products by High Performance Liquid Chromatography with Solid Phase Extraction Using Metal-Organic Framework as Sorbent

牛灿杰 1叶素丹 1朱千聪 1胡玉霞1
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作者信息

  • 1. 浙江经贸职业技术学院,浙江 杭州 310012
  • 折叠

摘要

采用溶剂热法合成新型金属有机骨架材料UiO-66-NH2,建立基于UiO-66-NH2的固相萃取-高效液相色谱同时检测水产品中5 种氟喹诺酮类药物残留的方法.样品经体积分数1.0%甲酸-乙腈溶液提取,正己烷脱脂,提取液旋蒸浓缩后,采用pH 8.0的氨水溶液复溶,经装有30 mg UiO-66-NH2 的固相萃取柱富集净化,6 mL 20%乙酸-甲醇溶液洗脱,氮吹近干复溶后,利用高效液相色谱-荧光检测器检测.在建立的实验条件下,5 种FQs在0.005~0.50 mg/L范围内线性关系良好,决定系数(R2)为0.999 9~1.0,回收率为81.4%~104.8%,相对标准偏差为1.29%~4.93%,检出限为0.21~2.05 μg/kg.制备的固相萃取柱可重复使用达5 次,绿色环保、经济成本低,所建立的方法具有良好的准确度、精密度、重现性及选择性,适用于水产品中多种痕量氟喹诺酮类药残的同时检测.

Abstract

A novel metal-organic framework(MOF)material,UiO-66-NH2,was synthesized using a solvothermal method.Subsequently,a high performance liquid chromatography(HPLC)method with solid phase extraction using UiO-66-NH2 was established for the simultaneous detection of five fluoroquinolone(FQ)residues in aquatic products.The sample was extracted with acetonitrile in 1.0%formic acid,degreased with n-hexane,and concentrated by rotary evaporation.The extract was then redissolved in aqueous ammonia solution at pH 8.0.The FQs were enriched and purified with a solid phase extraction(SPE)column filled with 30 mg of UiO-66-NH2 using 6 mL of 20%acetic acid-methanol solution as the eluent.The collected eluate was blown to dryness under nitrogen,redissolved and detected by HPLC with a fluorescence detector.Under the established experimental conditions,good linear relationships were achieved for the five FQs in the concentration range of 0.005-0.50 mg/L,with determination coefficients(R2)of 0.999 9-1.0.The recovery rates ranged from 81.4%to 104.8%with relative standard deviation(RSD)of 1.29%-4.93%,and the limits of detection(LOD)were in the range of 0.21-2.05 μg/kg.The prepared SPE column could be reused up to five times,which was environmentally friendly and cost-effective.The established method had good accuracy,precision,reproducibility,and selectivity,and was suitable for the simultaneous detection of various trace FQ residues in aquatic products.

关键词

金属有机骨架/固相萃取/高效液相色谱/水产品/氟喹诺酮类药物

Key words

metal-organic framework/solid phase extraction/high performance liquid chromatography/aquatic products/fluoroquinolones

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出版年

2025
食品科学
北京食品科学研究院

食品科学

北大核心
影响因子:1.327
ISSN:1002-6630
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