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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
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摘要 采用溶剂热法合成新型金属有机骨架材料UiO-66-NH_(2),建立基于UiO-66-NH_(2)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-NH_(2)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(R^(2))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0.21~2.05μg/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。 A novel metal-organic framework(MOF)material,UiO-66-NH_(2),was synthesized using a solvothermal method.Subsequently,a high performance liquid chromatography(HPLC)method with solid phase extraction using UiO-66-NH_(2) 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-NH_(2) 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(R^(2))of 0.9999–1.0.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 0.21–2.05μg/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.
作者 牛灿杰 叶素丹 朱千聪 胡玉霞 NIU Canjie;YE Sudan;ZHU Qiancong;HU Yuxia(Zhejiang Institute of Economic and Trade,Hangzhou 310012,China)
出处 《食品科学》 EI CAS 北大核心 2025年第3期222-229,共8页 Food Science
基金 浙江省基础公益研究计划项目(自然科学基金探索项目)(LTGC24C200003) 浙江经贸职业技术学院省属高校基本科研业务费专项(23SBYB01) 浙江省教育厅科研资助项目(Y202353372) 教育部高等学校科学研究发展中心《虚拟仿真技术在职业教育教学中的创新应用》专项(ZJXF2022188)。
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 metal-organic framework solid phase extraction high performance liquid chromatography aquatic products fluoroquinolones
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