为获得β-内酰胺类抗生素多残留检测样品净化和富集预处理所需选择性固相萃取填料,本文对采取沉淀聚合方法制备苯唑西林印迹微球进行研究,并对合成的微球进行分子识别特性研究。在反应温度60℃,反应时间24h条件下,优化的合成反应参数是:模板苯唑西林、功能单体丙烯酰胺与交联剂二甲基丙烯酸乙二醇酯的用量分别为1、4和20mmol(物质的量比为1∶4∶20),溶剂甲醇100mL,引发剂偶氮二异丁腈5mg。合成出的苯唑西林印迹微球具有两类性质不同的吸附位点,低亲和性吸附位点平衡常数K和最大表观吸附量Q分别为10.846mmol/L和418.23μmol/g,高亲和性吸附位点平衡常数K和最大表观吸附量Q分别为2.627mmol/L和137.68μmol/g。印迹聚合物重复使用次数不少于9次,对β-内酰胺类抗生素青霉素-G、头孢哌酮和头孢唑林的吸附量达模板吸附量的95%、58%和96%,对加标牛奶样品的净化效果表明其具有直接用作固相萃取柱填料的潜力。
The selective sorbents, oxacillin-imprinted microspheres, used in solid-phase extraction cartridge are needed to isolate the beta lactam antibiotics from samples. A method was developed to prepare these microspheres by precipitation polymerization, and the molecular recognition characteristics of these microspheres were studied. The optimized synthesis parameters were as follows. The amounts of template oxacillin, functional monomer acrylamide and crosslinker ethylene-dimethacrylate were 1, 4 and 20 mmol (molar ratio of 1 : 4: 20); the solvent methanol was 100 mL, and initiator azodiisobutyronitrile was 5 rag. The polymerization was carried out at 60 ℃ for 24 h. There were two classes of binding sites in the oxacillin-imprinted microspheres. The dissociation constant of low affinity's binding site was 10.846 mmol/L, and the max apparent binding capacity was 418.23 μmol/g. The dissociation constant of high affinity's binding site was 2.627 retool/L, and the max apparent binding capacity was 137.68 μmol/g. The adsorption quantity of the microspheres to penicillin-G, cefoperazone and cefazolin were 95%, 58% and 96% of that template. The molecularly imprinted polymers could be reused nine times without significant decrease on adsorption properties. The result of spiked milk sample proved that the oxacillin-imprinted microspheres could be directly used as the sorbents of solid phase extraction cartridge.