分子印迹固相萃取-HPLC法检测食品中4种喹诺酮类抗生素

Determination of four quinolones antibiotics in food by molecularly imprinted solid phase extraction combined with HPLC

目的:建立检测鸡肉鸡蛋中4种喹诺酮类抗生素的分子印迹固相萃取-高效液相色谱(紫外检测器)的分析方法。方法:采用乳液聚合法制备诺氟沙星印迹聚合物(MIPs),采用扫描电镜和红外光谱对印迹聚合物进行表征。采用印迹聚合物为固相萃取剂,优化了影响萃取效率的参数包括淋洗剂的种类及用量、洗脱剂的种类及用量。结果:在优化的实验条件下,4种喹诺酮类抗生素在1.5～100μg/mL浓度范围内呈良好线性关系(r> 0.992),方法的检出限(S/N=3)为0.04～0.4μg/mL,鸡肉鸡蛋样品中喹诺酮类抗生素的加标回收率为82.0%～96.0%,相对标准偏差(RSD)范围在3.9%～6.5%。结论:该方法快速、灵敏、可靠,能够满足食品中喹诺酮类抗生素多残留检测要求。

Objective :To develope a method for the determination of four kinds of quinolones antibiotics in food by molecularly imprinted solid phase extraction(MISPE)and high performance liquid chromatography-ultraviolet detector(HPLC-UV). Methods :A norfloxacin molecularly imprinted polymers(MIPs)was prepared via emulsion polymerization. The MIPs were characterized by scanning electron microscopy(SEM)and Fourier transform infrared spectrometry(FTIR).The MIPs were applied as solid-phase extraction materials to extract quinolones antibiotics in chicken meat and eggs. The parameters affecting the performance of extraction including the type and dosage of the elution as well as the type and dosage of the washing solvent were optimized. Results :Under the optimum conditions,good linear relationships in the range of 1.5 ~ 100 μg/mL were obtained with correlation coefficients(r)greater than 0.992. The detection limit(S/N=3)of the method was 0.04 ~ 0.4 μg/mL. The recoveries of quinolones antibiotics from the spiked chicken meat and eggs were 82.0% ~ 96.0% and the ranges of relative standard deviations(RSDs)were 3.9% ~ 6.5%. Conclusion :This method is rapid,sensitive,reliable,and can meet the requirements of multiple quinolones antibiotic residues determination in foods.