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Determination of nitrofuran and chloramphenicol residues by high resolution mass spectrometry versus tandem quadrupole mass spectrometry

机译:高分辨率质谱与串联四极杆质谱法测定硝基呋喃和氯霉素残留量

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摘要

An ultra-high performance liquid chromatography based method, coupled to high resolution mass spectrometry (UHPLC-HRMS), was developed to permit the detection and quantification of various nitrofuran and chloramphenicol residues in a number of animal based food products. This method is based on the hydrolysis of covalently bound metabolites and derivatization with 2-nitrobenzaldehyde. Clean-up is achieved by a liquid/liquid and a reversed phase/solid phase extraction. Not only are the four conventional nitrofurans (nitrofurantoin, furazolidone, nitrofurazone and furaltadone) detected, but also nifursol, nitrovin and nifuroxazide. Furthermore, an underivatizable nitrofuran (nifurpirinol) and another banned drug (chloramphenicol) can be quantified as well. The compounds are detected in the form of their precursor ions, [M + H](+) and [M - H] , respectively. The mass resolving power of 70,000 FWHM, and the applied mass window ensure sufficient selectivity and sensitivity. Confirmation is obtained by monitoring the HRMS resolved product ions which were derived from the unit-mass resolved precursor ions. The multiplexing capability of the utilized Orbitrap instrument provides not only highly selective, but also sensitive confirmatory signals. This method has been validated according to the CD 2002/657/EC for the following matrices: muscle, liver, kidney, fish, honey, eggs and milk. (C) 2015 Elsevier B.V. All rights reserved.
机译:开发了一种基于超高效液相色谱的方法,并结合了高分辨率质谱(UHPLC-HRMS),可检测和定量多种动物食品中各种硝基呋喃和氯霉素的残留量。该方法基于共价结合的代谢物的水解和2-硝基苯甲醛的衍生化。通过液/液和反相/固相萃取来实现净化。不仅检出了四种常规的硝基呋喃(呋喃妥因,呋喃唑酮,硝基呋喃酮和呋喃他酮),而且还检测了尼呋索尔,硝化氮和尼呋拉嗪。此外,还可以对可衍生化的硝基呋喃(硝呋比诺尔)和另一种禁用药物(氯霉素)进行定量。分别以其前体离子[M + H](+)和[M-H]的形式检测化合物。 70,000 FWHM的质量分辨能力和应用的质量窗口确保了足够的选择性和灵敏度。通过监测源自单位质量分辨前体离子的HRMS分辨产物离子来获得确认。所利用的Orbitrap仪器的多路复用能力不仅提供了高选择性的信号,而且还提供了敏感的确认信号。根据CD 2002/657 / EC,该方法已针对以下基质进行了验证:肌肉,肝脏,肾脏,鱼,蜂蜜,鸡蛋和牛奶。 (C)2015 Elsevier B.V.保留所有权利。

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