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液相色谱-串联质谱联用结合选择性分子印迹固相萃取法测定食品中的痕量四环素类抗生素

Determination of trace tetracycline antibiotics in foodstuffs by liquid chromatography-tandem mass spectrometry coupled with selective molecular-imprinted solid-phase extraction.

作者信息

Jing Tao, Gao Xiao-Dan, Wang Peng, Wang Yan, Lin Yan-Fei, Hu Xiao-Zhong, Hao Qiao-Lin, Zhou Yi-Kai, Mei Su-Rong

机构信息

MOE Key Laboratory of Environment and Health, Institute of Environmental Medicine, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, #13 Hangkong Road, Wuhan, Hubei, 430030, China.

出版信息

Anal Bioanal Chem. 2009 Apr;393(8):2009-18. doi: 10.1007/s00216-009-2641-z. Epub 2009 Feb 12.

Abstract

A rapid, specific, and sensitive method has been developed using molecularly imprinted polymers (MIPs) as solid-phase extraction sorbents for extraction of trace tetracycline antibiotics (TCs) in foodstuffs. MIPs were prepared by precipitation polymerization using tetracycline as the template. Under the optimal condition, the imprinting factors for MIPs were 4.1 (oxytetracycline), 7.0 (tetracycline), 7.4 (chlortetracycline), 7.7 (doxycycline), respectively. Furthermore, the performance of MIPs as solid-phase extraction sorbents was evaluated and high extraction efficiency of molecularly imprinted solid-phase extraction (MISPE) procedure was demonstrated. Compared with commercial sorbents, MISPE gave a better cleanup efficiency than C18 cartridge and a higher recovery than Oasis HLB cartridge. Finally, the method of liquid chromatography-tandem mass spectrometry coupled with molecular-imprinted solid-phase extraction was validated in real samples including lobster, duck, honey, and egg. The spiked recoveries of TCs ranged from 94.51% to 103.0%. The limits of detection were in the range of 0.1-0.3 microg kg(-1).

摘要

已开发出一种快速、特异且灵敏的方法,该方法使用分子印迹聚合物(MIPs)作为固相萃取吸附剂,用于提取食品中的痕量四环素类抗生素(TCs)。以四环素为模板,通过沉淀聚合法制备MIPs。在最佳条件下,MIPs对土霉素、四环素、金霉素、强力霉素的印迹因子分别为4.1、7.0、7.4、7.7。此外,对MIPs作为固相萃取吸附剂的性能进行了评估,并证明了分子印迹固相萃取(MISPE)程序具有较高的萃取效率。与市售吸附剂相比,MISPE的净化效率优于C18柱,回收率高于Oasis HLB柱。最后,采用液相色谱-串联质谱联用分子印迹固相萃取的方法在包括龙虾、鸭肉、蜂蜜和鸡蛋在内的实际样品中进行了验证。TCs的加标回收率在94.51%至103.0%之间。检测限在0.1 - 0.3 μg kg⁻¹范围内。

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