首页|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

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

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

metal-organic frameworksolid phase extractionhigh performance liquid chromatographyaquatic productsfluoroquinolones

牛灿杰、叶素丹、朱千聪、胡玉霞

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浙江经贸职业技术学院,浙江 杭州 310012

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

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
年,卷(期):2025.46(3)