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目的:采用表面引发原子转移自由基聚合(SI-ATRP)技术合成了氯霉素表面分子印迹聚合物并应用于动物源食品中痕量氯霉素富集分析。方法:以2-溴异丁酰溴为引发剂,氯霉素为模板分子,甲基丙烯酸二乙基氨基乙酯(DEAEM)为功能单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,CuBr/2,2’-联吡啶(Bpy)为催化剂,在室温下采用SI-ATRP将模板分子氯霉素印迹到硅胶表面,制得了氯霉素表面分子印迹聚合物。采用静态吸附实验和选择性实验研究了分子印迹聚合物(MIPs)对氯霉素的结合性能与分子识别特性。结果:MIPs对氯霉素最大吸附量为0.48 mmol·g-1,相对于结构类似物琥珀酸氯霉素、甲砜霉素和氟苯尼考的选择性系数分别为2.51、4.39和1.40,相对选择性系数分别为1.68、3.40和1.92。MIPs与固相萃取联用,对牛肉样品进行了加标回收试验,平均回收率为92.4%~98.7%,相对标准偏差为5.2%~6.2%,方法的检出限可达10 ng·g-1。结论:该MIPs具有良好的吸附选择性和较高的吸附容量且结合速率快,与市售C18固相萃取小柱相比,该MIPs更适合作为固相萃取吸附剂对动物源食品中的痕量氯霉素残留进行富集分析。
OBJECTIVE: Chloramphenicol surface molecularly imprinted polymers were synthesized by surface-initiated atom transfer radical polymerization (SI-ATRP) and applied to the determination of trace chloramphenicol in animal-derived foods. Methods: 2-bromoisobutyryl bromide as initiator, chloramphenicol as template, diethylaminoethyl methacrylate (DEAEM) as functional monomer and ethylene glycol dimethacrylate (EDMA) as Chloramphenicol surface molecularly imprinted polymer was prepared by using Si-ATRP and CuBr / 2,2’-bipyridyl (Bpy) as catalyst. The adsorption properties and molecular recognition properties of MIPs to chloramphenicol were studied by static adsorption experiments and selective experiments. Results: The maximum adsorption of chloramphenicol by MIPs was 0.48 mmol · g-1. The selectivity coefficients of MIPs against chloramphenicol succinate, thiamphenicol and florfenicol were 2.51, 4.39 and 1.40, respectively. The relative selectivity coefficients were 1.68, 3.40 and 1.92, respectively. MIPs and solid-phase extraction, the beef samples were spiked recovery test, the average recovery was 92.4% to 98.7%, the relative standard deviation of 5.2% to 6.2%, the detection limit of the method up to 10 ng · g- 1. Conclusion: The MIPs have good adsorption selectivity and high adsorption capacity and fast binding rate. Compared with commercially available C18 solid phase extraction cartridges, the MIPs are more suitable as solid phase extraction adsorbents for animal-derived foodstuffs Quantity of chloramphenicol residues for enrichment analysis.