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采用分子印迹分散固相萃取与 LC-MS/MS 法测定猪肉中的大环内酯类抗生素残留。

Determination of macrolide antibiotics residues in pork using molecularly imprinted dispersive solid-phase extraction coupled with LC-MS/MS.

机构信息

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

Guangdong Provincial Key Laboratory of Veterinary Pharmaceutics Development and Safety Evaluation, South China Agricultural University, Guangzhou, China.

出版信息

J Sep Sci. 2018 Mar;41(5):1138-1148. doi: 10.1002/jssc.201700973. Epub 2018 Jan 25.

DOI:10.1002/jssc.201700973
PMID:29280550
Abstract

A class-specific macrolide molecularly imprinted polymer was synthesized by precipitation polymerization using tulathromycin as the template and methacrylic acid as the functional monomer. The polymers revealed different specific adsorption and imprinting factor for macrolides with different spatial arrangement of side chains as well as lactonic ring size. And the molecularly imprinted polymer possessed maximum adsorption capacity (54.1 mg/g) and highest imprinting factor (2.4) toward 15-membered ring azithromycin. On the basis of molecularly imprinted polymer dispersive solid-phase extraction, a rapid, selective, and reproducible method for simultaneous determination of seven macrolide antibiotics residues in pork was established by using liquid chromatography with tandem mass spectrometry. At spiking levels of 5, 10, 25, and 100 μg/kg, average recoveries of seven macrolides ranged from 68.6 to 95.5% with intraday and interday relative standard deviations below 8%. The limits of detection and limits of quantification were 0.2-0.5 and 0.5-2.0 μg/kg, respectively.

摘要

采用沉淀聚合法,以酒石酸泰乐菌素为模板分子、甲基丙烯酸为功能单体合成了一种大环内酯类分子印迹聚合物。该聚合物对侧链空间排列和内酯环大小不同的大环内酯类化合物表现出不同的特异吸附和印迹因子。对于 15 元环阿奇霉素,分子印迹聚合物具有最大的吸附容量(54.1mg/g)和最高的印迹因子(2.4)。基于分子印迹聚合物分散固相萃取,建立了一种快速、选择性和重现性好的液相色谱-串联质谱法同时测定猪肉中 7 种大环内酯类抗生素残留的方法。在 5、10、25 和 100μg/kg 的加标水平下,7 种大环内酯类抗生素的平均回收率在 68.6%至 95.5%之间,日内和日间相对标准偏差均低于 8%。检测限和定量限分别为 0.2-0.5 和 0.5-2.0μg/kg。

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