喹乙醇残留标识物分子印迹材料的制备及应用

发布时间：2018-07-12 11:25

本文选题：喹VA啉-2-羧酸 + 3-甲基喹VA啉-2-羧酸　；参考：《天津科技大学》2012年硕士论文

【摘要】：喹VA啉类是人工合成的动物抗菌促生长药物,其中喹乙醇(OLA)和卡巴氧(CBX)(?)应用最广的品种,在动物基体中的残留标识物分别为3-甲基喹VA(?)羧酸(MQCA)和喹嗯啉-2-羧酸(QCA)。本论文首先合成MQCA,然后以MQCA为模板分子,活化硅球为表面载体,3-氨基丙基三乙氧基硅烷(APTES)为功能单体,四乙氧基硅烷(TEOS)为交联剂,采用表面分子印迹和溶胶-凝胶相结合的技术制备了MQCA分子印迹聚合物。通过红外光谱和吸附试验对聚合物进行了表征,吸附试验结果表明聚合物传质速度快、吸附容量大对QCA和MQCA均有高选择性。以此聚合物为固相萃取吸附材料,建立了动物源性食品中QCA和MQCA戈留的在线固相萃取与高效液相色谱仪联用检测方法,并对影响测定结果的上样溶剂配比,pH值,上样速度及洗脱时间等主要实验参数进行了优化。在上样流速为2.0mL min-1、上样体积为50mL条件下,对1.0μg L-1QCA和MQCA勺混合标准溶液(pH5.0,甲醇含量1%)进行富集,富集倍数分别达到1349和1046；九次重复测定的相对标准偏差(RSD,%)小于8%；检出限(S/N=3)分别为0.8和2.0ng L-1；线性范围(r20.99)分别为0.03-40μg L-1和0.04-40μg L-1。同时对猪肉样品中的痕量QCA和MQCA进行了检测分析。样品前处理方法简单,酸性水解液释放待分析物后仅用一步乙腈提取就能满足测定要求,不需要进步的样品净化。通过对检测为空白的新鲜样品进行浓度为2.0ng g-1,4.0ng g-1,8.0ng g-1的添加,以所建立的分析方法进行富集测定,结果在三个添加浓度下样品中QCA和MQCA的回收率为67%-80%,从而证明了所建立检测方法的可行性。
[Abstract]:Quinavalin is a synthetic antibacterial and growth-promoting drug in animals, in which quindoquindox (Ola) and carbamoxime (CBX) (?) The residues in animal matrix of the most widely used species are 3-methylquine VA (?) Carboxylic acid (MQCA) and quinoline-2-carboxylic acid (QCA). In this thesis, MQCA was synthesized firstly, and then the activated silica spheres were used as the surface support, and tetraethoxy silane (TEOS) as crosslinking agent. MQCA molecularly imprinted polymers were prepared by surface molecular imprinting and sol-gel techniques. The polymer was characterized by infrared spectroscopy and adsorption test. The results showed that the mass transfer rate of the polymer was fast and the adsorption capacity was high selectivity to both QCA and MQCA. Using this polymer as solid phase extraction adsorption material, an on-line solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) method for the determination of QCA and MQCA-Goru in animal-derived food was established. The main experimental parameters such as sample rate and elution time were optimized. The mixed standard solution of 1.0 渭 g L-1QCA and MQCA (pH 5.0, methanol content 1%) was enriched at a flow rate of 2.0 mL min-1 and a volume of 50 mL. The enrichment times were 1349 and 1046, respectively, and the relative standard deviation (RSD) of nine times repeated determination was less than 8%. The detection limit (S / N ~ (3) was 0. 8 and 2.0ng L ~ (-1), the linear range (r _ (20.99) was 0.03-40 渭 g / L ~ (-1) and 0.04-40 渭 g / L ~ (-1), respectively. At the same time, trace QCA and MQCA in pork samples were analyzed. The method of sample pretreatment is simple. After the acid hydrolysate releases the analyte, only one step acetonitrile can be extracted to meet the determination requirements, and no progressive sample purification is needed. The fresh samples with blank detection were enriched and determined by adding 4.0 ng / g ~ (-1) 2.0ng g ~ (-1) or 8.0 ng / g ~ (-1) to 2.0ng g ~ (-1). Results the recoveries of QCA and MQCA in the samples were 67-80, which proved the feasibility of the established method.
【学位授予单位】：天津科技大学
【学位级别】：硕士
【学位授予年份】：2012
【分类号】：R318.08

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