School of Food Science and Engineering, Shandong Academy of Sciences, Qilu University of Technology, Jinan, P. R. China.
J Sep Sci. 2020 Jun;43(11):2172-2179. doi: 10.1002/jssc.201901285. Epub 2020 Mar 29.
The present work reported a novel hydrophilic and selective solid-phase microextraction fiber by improved multiple co-polymerization method immobilization of tetracycline molecularly imprinted polymer on a stainless steel wire and directly coupled with high-performance liquid chromatography for sensitive determination of trace tetracyclines residues in animal derived foods. The developed molecularly imprinted polymer coated solid-phase microextraction fibers were characterized through scanning electron microscopy, Fourier transfer infrared spectroscopy, thermogravimetric analysis, and adsorption experiments, the fiber with cross-linked and porous structure was observed and high thermal and chemical stability. The maximum adsorption capacity of this fiber with good selectivity reached 2.35 µg/mg in aqueous matrices, and showed good repeatability (relative standard deviation ≤ 6.6%, n = 5) and satisfying reproducibility between fiber to fiber (relative standard deviation ≤ 7.8%, n = 5). Under the optimized solid-phase microextraction conditions, satisfactory linearity (5-1000 µg/L) and detection limits (0.38-0.72 µg/kg, S/N = 3) for all the tetracyclines were obtained. The practicality of this method was proved by adding tetracycline, oxytetracycline at three levels to milk, chicken, and fish samples with good recoveries of 77.3-104.4%.
本工作报道了一种新型的亲水和选择性固相微萃取纤维，通过改进的多次共聚方法将四环素分子印迹聚合物固定在不锈钢丝上，并与高效液相色谱直接耦合，用于灵敏测定动物源性食品中的痕量四环素残留。通过扫描电子显微镜、傅里叶变换红外光谱、热重分析和吸附实验对所开发的分子印迹聚合物涂层固相微萃取纤维进行了表征，观察到纤维具有交联和多孔结构，具有较高的热稳定性和化学稳定性。这种纤维具有良好选择性，在水基基质中的最大吸附容量达到 2.35µg/mg，具有良好的重现性（相对标准偏差≤6.6%，n=5）和纤维间的可重复性（相对标准偏差≤7.8%，n=5）。在优化的固相微萃取条件下，所有四环素均获得了令人满意的线性（5-1000µg/L）和检测限（0.38-0.72µg/kg，S/N=3）。该方法通过向牛奶、鸡肉和鱼肉样品中添加四环素和土霉素三种水平进行了实际应用，回收率为 77.3-104.4%。
