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一种灵敏、选择性的印迹固相萃取与 HPLC 相结合,用于同时检测动物肌肉中的痕量喹喔啉-2-羧酸和甲基-3-喹喔啉-2-羧酸。

A sensitive and selective imprinted solid phase extraction coupled to HPLC for simultaneous detection of trace quinoxaline-2-carboxylic acid and methyl-3-quinoxaline-2-carboxylic acid in animal muscles.

机构信息

Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin University of Science and Technology, Tianjin 300457, China.

出版信息

Food Chem. 2013 Aug 15;139(1-4):274-80. doi: 10.1016/j.foodchem.2013.02.007. Epub 2013 Feb 16.

Abstract

A new molecularly imprinted polymer (MIP), selective for major metabolites of quinoxaline-1,4-dioxides, was prepared through bulk polymerisation using quinoxaline-2-carboxylic acid (QCA) as template, diethylaminoethylmethacrylate as functional monomer and ethylene glycol dimethacrylate as cross-linker in tetrahydrofuran. The synthesised MIP was characterised by Fourier transform infrared and adsorption experiments. MIP exhibited high affinity, fast kinetics for QCA and good selectivity for QCA and methyl-3-quinoxaline-2-carboxylic acid (MQCA). MIP obtained was used as a selective sorbent for molecularly imprinted solid phase extraction (MISPE) coupled with HPLC to detect QCA and MQCA. Under the optimal conditions, the limits of detection (S/N=3) of porcine, chicken and fish muscles were 0.1, 0.3, 0.1 μg/kg for QCA and 0.2, 0.3, 0.1 μg/kg for MQCA, respectively and good recoveries were obtained in the range from 60.0 to 119.4%. These results indicated the MISPE-HPLC procedure could be successfully used for the determination QCA and MQCA in animal muscles.

摘要

一种新的分子印迹聚合物(MIP),对喹喔啉-1,4-二酮的主要代谢物具有选择性,通过本体聚合制备,以喹喔啉-2-羧酸(QCA)为模板,二乙基氨乙基甲基丙烯酸酯为功能单体,乙二醇二甲基丙烯酸酯为交联剂,在四氢呋喃中进行。所合成的 MIP 通过傅里叶变换红外和吸附实验进行了表征。MIP 对 QCA 具有高亲和力、快速动力学和对 QCA 和甲基-3-喹喔啉-2-羧酸(MQCA)的良好选择性。所得 MIP 用作分子印迹固相萃取(MISPE)与 HPLC 结合的选择性吸附剂,用于检测 QCA 和 MQCA。在最佳条件下,猪、鸡和鱼肉中 QCA 的检出限(S/N=3)分别为 0.1、0.3 和 0.1μg/kg,MQCA 的检出限分别为 0.2、0.3 和 0.1μg/kg,回收率在 60.0%至 119.4%之间。这些结果表明,MISPE-HPLC 程序可成功用于动物肌肉中 QCA 和 MQCA 的测定。

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