羟基有机网络材料用于牛奶中氟喹诺酮类抗生素的检测

Application of the novel organic network material for the detection of fluoroquinolone antibiotics in milk

牛奶中氟喹诺酮类抗生素残留可增加居民膳食暴露风险,发展其检测方法是食品安全的重要需求.本文以1,3,5-三乙炔苯和2,4,6-三碘苯酚为单体,在30℃的温和条件下通过Sonogashira耦合反应合成了羟基有机网络材料,并对其形貌、结构和疏水性进行了表征.由于π-π、氢键和疏水作用,该材料能够高效保留牛奶基质中的氟喹诺酮类抗生素.将其作为固相萃取(SPE)吸附剂,结合高效液相色谱荧光检测器对管尖SPE条件进行优化,提出了牛奶中氧氟沙星、环丙沙星和恩诺沙星样品前处理的新方法.在0.4~100μg/kg的浓度范围内,R^(2)≥0.9992,线性关系良好,检出限为0.15~1.2μg/kg,加标回收率和相对标准偏差分别为89.6%~103.5%和1.3%~5.9%,适用于牛奶样品中三种氟喹诺酮类抗生素的检测.

The residues of fluoroquinolone antibiotics in milk increase the risk of dietary exposure.The development of detection technology is an important guarantee of food safety.In this work,1,3,5-triacetylbenzene and 2,4,6-triiodophenol were selected as monomers to synthesize new organic network materials based on Sonogashira coupling reaction under moderate condition of 30℃.Morphology,structure and hydrophobicity of the prepared material were characterized.Due to theπ-π,hydrogen bonding and hydrophobic interaction,fluoroquinolone antibiotics in milk can be absorbed efficiently on the material.As an adsorbent of solid phase extraction(SPE),the pipette-tip SPE conditions were optimized combined with high performance liquid chromatography coupled with fluorescence detector,and the novel method for the detection of fluoroquinolone antibiotics in milk was established.The linear range was 0.4–100μg/kg,and R^(2)≥0.9992 showed the good linear relationship.The detection limit was 0.15–1.2μg/kg.The recoveries and relative standard deviations were 89.6%–103.5%and 1.3%–5.9%,respectively.It was suitable for the determination of fluoroquinolone antibiotics in milk samples.