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投稿时间:2024-09-19
投稿时间:2024-09-19
中文摘要: 针对禽蛋中多种氟喹诺酮类(fluoroquinolones,FQs)药物残留量并存的实际问题,建立7 种氟喹诺酮类药物残留固相萃取-高效液相色谱法,用于鸡蛋、鸭蛋、鹅蛋中多重药物残留的分析。试验结果表明:除脂条件为8 000 r/min 离心10 min,C18 固相萃取柱净化富集,5.0%乙腈+0.3%磷酸水溶液 (pH4.0) 为流动相,FQs 回收率最高;在优化条件下,7 种FQs 在22 min 内完全分离,7 种FQs 浓度(10~2 000 μg/kg)与相应峰面积呈良好线性关系,相关系数R2≥0.999 0,检测限范围为1.5~6.7 μg/kg。对阴性鸡蛋、鸭蛋、鹅蛋进行7 种氟喹诺酮药物10.0、50.0 μg/kg 加标回收试验,方法回收率为82.0%~103.1%,相对标准偏差小于6.3%(n=6)。该方法分析速度快、灵敏度高、稳定性好,可用于禽蛋中7 种FQs 药物残留的同时快速定量检测。
Abstract:In view of the residues of multiple fluoroquinolones (FQs) in poultry eggs, a solid-phase extractionhigh performance liquid chromatography method was established. This method was then used for detecting residues of multiple in chicken eggs, duck eggs, and goose eggs. The results showed that the highest recovery of FQs was achieved when the time of centrifugation for lipid removal was 8 000 r/min 10 min and purification and enrichment were performed on the C18 column with the mobile phase of 5.0% acetonitrile+0.3% phosphoric acid solution (pH4.0). Under the optimized working conditions, the seven FQs were completely separated within 22 min. There was a good linear relationship between the concentrations of the seven FQs and the corresponding peak areas within the concentration range of 10-2 000 μg/kg, with R2≥0.999 0. The limit of detection of the established method for residues of the seven FQs ranged from 1.5-6.7 μg/kg. The spiked recovery of 10.0,50.0 μg/kg FQs in negative chicken eggs, duck eggs, and goose eggs were 82.0%-103.1%, and the relative standard deviation was less than 6.3% (n=6). This method was fast, sensitive, and stable and can be used for simultaneously and quantitatively detecting the residues of seven FQs in poultry eggs.
keywords: solid-phase extraction-high performance liquid chromatography fluoroquinolones veterinary drug residues rapid detection poultry eggs food safety
文章编号:202507020 中图分类号: 文献标志码:
基金项目:浙江省基础公益研究计划项目(LQ23C200006);浙江省科技计划项目(2022C02049、2021C02061)
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