采用沉淀聚合法,以诺氟沙星为模板分子,合成了对氟喹诺酮类(FQs)抗生素特异性识别的分子印迹聚合物(MIPs),其印迹因子为3.17,亲和位点总数为3.27μmol/g。以该MIPs做为固相萃取柱填料,建立了分子印迹固相萃取-高效液相色谱检测蜂蜜中三种FQs抗生素残留的方法。与Oasis HLB固相萃取柱相比,该分子印迹固相萃取柱(MISPE)具有更好的净化能力和更高的富集效率。最佳条件下,三种FQs抗生素的线性范围为0.125~12.5mg/kg,相关系数均大于0.999。方法的检出限(S/N=3)为9~12μg/kg,三种FQs抗生素的加标回收率为96.5%~104.1%,相对标准偏差不高于6.2%(n=5)。该方法有望用于蜂蜜中FQs抗生素残留的常规检测。
In this study,molecularly imprinted polymers(MIPs)with specific recognition for the fluoroquinolones(FQs)antibiotics were prepared by precipitation polymerization using norfloxacin as the template.The imprinted factor was 3.17and the total amount of the immobilized ligand was 3.27μmol/ g.With the MIPs as solid phase extraction(SPE)sorbent,a molecularly imprinted solid-phase extraction coupled with high performance liquid chromatography(MISPE-HPLC)was established to determine three FQs antibiotics in honey samples.Compared with the commercial Oasis HLB cartridge,the MISPE method gave a better cleanup efficiency and a higher recovery.Under the optimized conditions,the linear range was 0.125~12.5mg/kg with the correlation coefficient greater than 0.999.The limits of detection were in the range of 9~12μg/kg(S/N=3).The recoveries of three FQs antibiotics in spiked samples were 96.5%~104.1% with the relative standard deviations lower than 6.2%(n=5).This method was suitable for routine analysis of FQs antibiotics residues in honey samples.