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采用分子印迹固相萃取与高效液相色谱法同时测定饲料中的喹喔啉-1,4-二氧化物。

Simultaneous determination of quinoxaline-1,4-dioxides in feeds using molecularly imprinted solid-phase extraction coupled with HPLC.

机构信息

National Reference Laboratory of Veterinary Drug Residues (SCAU), College of Veterinary Medicine, South China Agricultural University, Guangzhou, China.

出版信息

J Sep Sci. 2013 Jan;36(2):301-10. doi: 10.1002/jssc.201200701. Epub 2012 Dec 10.

Abstract

A simple, selective, and reproducible molecularly imprinted SPE coupled with HPLC method was developed for monitoring quinoxaline-1,4-dioxides in feeds. Molecularly imprinted polymers were synthesized in methanol using mequindox (MEQ) as template molecule and acrylamide as functional monomer by bulk polymerization. Under the optimum SPE conditions, the novel polymer sorbents can selectively extract and enrich carbadox, MEQ, quinocetone, and cyadox from a variety of feeds. The molecularly imprinted SPE cartridge was better than nonimprinted, C(18) , and HLB cartridges in terms of both recovery and precision. Mean recoveries of four quinoxaline-1,4-dioxides from six kinds of feeds spiked at 1.0, 10, and 100 mg/kg ranged between 75.2 and 94.7% with RSDs of less than 10%. The decision limits (CCαs) and the detection capabilities (CCβs) of four analytes were 0.15-0.20 mg/kg and 0.44-0.56 mg/kg, respectively. The class selectivity of the polymers was evaluated by checking three drugs with different molecular structures to that of MEQ.

摘要

建立了一种简单、选择性好、重现性强的分子印迹固相萃取(MISPE)-高效液相色谱(HPLC)方法,用于监测饲料中的喹噁啉-1,4-二氧化物。采用本体聚合法,以马兜铃酸(MEQ)为模板分子,丙烯酰胺为功能单体,在甲醇中合成了分子印迹聚合物。在最佳 SPE 条件下,新型聚合物吸附剂可以从多种饲料中选择性地提取和富集卡巴多、MEQ、喹乙醇和潮霉素。在回收率和精密度方面,分子印迹 SPE 柱均优于非印迹柱、C18 柱和 HLB 柱。四种喹噁啉-1,4-二氧化物从六种添加浓度为 1.0、10 和 100 mg/kg 的饲料中的平均回收率在 75.2%至 94.7%之间,相对标准偏差(RSD)小于 10%。四种分析物的决策限(CCαs)和检测能力(CCβs)分别为 0.15-0.20 mg/kg 和 0.44-0.56 mg/kg。通过检查三种与 MEQ 具有不同分子结构的药物,评估了聚合物的类选择性。

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