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摘要:以甲基丙烯酸(MAA)为功能单体,以乙二醇二甲基丙烯酸酯(EGDMA)为交联剂,以乙腈为溶剂,采用沉淀聚合法合成氯霉素(chloramphenicol, CAP)分子印迹聚合物(CAP-MIPs),氯霉素、功能单体与交联剂比例1:4:24,聚合温度60℃,制备出性能优良的CAP-MIPs。 将洗脱后的氯霉素分子印迹聚合物作为固相萃取填料制成固相萃取柱,对萃取条件进行优化,5 mL乙腈活化柱子;3 mL10%的甲醇水溶液上样;2 mL30%的乙腈水作为淋洗液;3 mL甲醇/乙酸(v/v, 9:1)洗脱。对20 μmol/mL CAP溶液回收率在93.6%。然后用最优条件的固相萃取柱对含痕量氯霉素的牛奶进行吸附,表明吸附率达89.5%。可以较好的用于实际生活中检测氯霉素残留。研究聚合物的吸附性能,分子印迹聚合物的吸附能力远大于非印迹聚合物。采用Scatchard 模型对分子印迹聚合物的吸附性能进行分析,通过计算截距和斜率得出,其最大表观吸附量为40.55 μmol/g。 关键词 氯霉素;分子印迹聚合物;吸附性能;Scatchard 模型;固相萃取
Abstract:In this paper, precipitation polymerization synthesis of chloramphenicol ( chloramphenicol, CAP ) molecularly imprinted polymer ( CAP - MIPs ), methacrylic acid ( MAA ) as functional monomer, ethylene glycol dimethacrylate ( EGDMA ) cross- linking agent with acetonitrile as a solvent, through several experiments, chloramphenicol, functional monomer and crosslinking agent ratio of 1:4:24, the polymerization temperature of 60℃, prepared by the excellent performance of the CAP - MIPS. Chloramphenicol molecularly imprinted polymer eluted as solid-phase extraction filler made of solid phase extraction column to optimize the extraction conditions, activation of the column in 5 mL of acetonitrile; 3mL10% methanol aqueous solution sample; 2mL30% acetonitrile and water as leaching lotion; 3mL of methanol / acetic acid (v/v, 9:1 ) as eluent. 93.6% the 20 μmol/mL CAP solution recovery. Milk containing trace amounts of chloramphenicol and optimal conditions for solid phase extraction column adsorption indicated that the adsorption rate of 89.5%. Can be used for the detection of chloramphenicol residues in real life. Study on the adsorption properties of polymer, adsorption ability of the imprinted polymer is far greater than the non-imprinted polymer. Scatchard model was applied to the analysis of adsorption properties of molecularly imprinted polymer, calculated by the intercept and slope, the maximum apparent adsorption quantity is 40.55 μ mol/g. Keywords Chloramphenicol Molecularly imprinted polymers Adsorption Scatchard model solid phase extraction |