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采用分子印迹聚合物整体柱选择性样品预处理分析牛奶样品中的氟喹诺酮类药物。

Selective sample pretreatment by molecularly imprinted polymer monolith for the analysis of fluoroquinolones from milk samples.

机构信息

Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.

出版信息

J Chromatogr A. 2010 Apr 2;1217(14):2075-81. doi: 10.1016/j.chroma.2010.02.011. Epub 2010 Feb 10.

Abstract

Water-compatible pefloxacin-imprinted monoliths synthesized in a water-containing system were used for the selective extraction of fluoroquinolones (FQs). The MIP monolith was synthesized by using methacrylic acid as the functional monomer, di(ethylene glycol) dimethacrylate as a cross-linker and methanol-water (10:3, v/v) as the porogenic solvent. The ability of the derivated MIP for selective recognition of FQs (ciprofloxacin, difloxacin, danofloxacin and enrofloxacin) and quinolones (flumequine, and oxolinic acid) was evaluated. The derivated monolith showed high selectivity and was able to distinguish between FQs and quinolones. A simple rapid and sensitive method using polymer monolith microextraction (PMME) based on the MIP monolith combined with HPLC with fluorescence detection was developed for the determination of four FQs from milk samples. Owing to the unique porous structure and flow-through channels in the network skeleton of the MIP monolith, phosphate buffer diluted milk samples were directly supplied to PMME; allowing non-specific bound proteins and other biological matrix to be washed out, and FQs to be selectively enriched. The limit of detection of the method was 0.4-1.6ng/mL and recovery was 92.4-98.2% with relative standard deviations less than 5.9%.

摘要

在含水体系中合成的水相容的培氟沙星印迹整体柱用于选择性萃取氟喹诺酮类药物(FQs)。MIP 整体柱是通过使用甲基丙烯酸作为功能单体、二乙二醇二甲基丙烯酸酯作为交联剂以及甲醇-水(10:3,v/v)作为致孔溶剂来合成的。衍生的 MIP 对 FQs(环丙沙星、二氟沙星、达氟沙星和恩诺沙星)和喹诺酮类(氟甲喹和恶喹酸)的选择性识别能力进行了评估。衍生的整体柱表现出高选择性,能够区分 FQs 和喹诺酮类药物。一种简单、快速和灵敏的方法,使用基于 MIP 整体柱的聚合物整体柱微萃取(PMME)结合 HPLC 荧光检测,用于从牛奶样品中测定四种 FQs。由于 MIP 整体柱的网络骨架中具有独特的多孔结构和贯穿通道,因此可以直接将磷酸盐缓冲液稀释的牛奶样品供应给 PMME;允许非特异性结合的蛋白质和其他生物基质被冲洗掉,并选择性地富集 FQs。该方法的检出限为 0.4-1.6ng/mL,回收率为 92.4-98.2%,相对标准偏差小于 5.9%。

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