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采用液相色谱-串联质谱法对禽肉中的β-内酰胺类抗生素(包括青霉素类、头孢菌素类和碳青霉烯类)进行综合分析。

Comprehensive analysis of ß-lactam antibiotics including penicillins, cephalosporins, and carbapenems in poultry muscle using liquid chromatography coupled to tandem mass spectrometry.

机构信息

RIKILT, Wageningen University and Research Centre, Akkermaalsbos 2, 6708WB, P.O. Box 230, 6700AE, Wageningen, The Netherlands,

出版信息

Anal Bioanal Chem. 2013 Sep;405(24):7859-74. doi: 10.1007/s00216-013-6804-6. Epub 2013 Feb 22.

DOI:10.1007/s00216-013-6804-6
PMID:23430185
Abstract

A comprehensive method for the quantitative residue analysis of trace levels of 22 ß-lactam antibiotics, including penicillins, cephalosporins, and carbapenems, in poultry muscle by liquid chromatography in combination with tandem mass spectrometric detection is reported. The samples analyzed for ß-lactam residues are hydrolyzed using piperidine in order to improve compound stability and to include the total residue content of the cephalosporin ceftifour. The reaction procedure was optimized using a full experimental design. Following detailed isotope labeling, tandem mass spectrometry studies and exact mass measurements using high-resolution mass spectrometry reaction schemes could be proposed for all ß-lactams studied. The main reaction occurring is the hydrolysis of the ß-lactam ring under formation of the piperidine substituted amide. For some ß-lactams, multiple isobaric hydrolysis reaction products are obtained, in accordance with expectations, but this did not hamper quantitative analysis. The final method was fully validated as a quantitative confirmatory residue analysis method according to Commission Decision 2002/657/EC and showed satisfactory quantitative performance for all compounds with trueness between 80 and 110% and within-laboratory reproducibility below 22% at target level, except for biapenem. For biapenem, the method proved to be suitable for qualitative analysis only.

摘要

本文报道了一种用于检测家禽肌肉中痕量 22 种β-内酰胺类抗生素(包括青霉素类、头孢菌素类和碳青霉烯类)残留的综合定量分析方法。该方法采用哌啶对样品进行水解,以提高化合物稳定性并包括头孢曲松的总残留含量。通过全因子实验设计对反应条件进行了优化。在详细的同位素标记、串联质谱研究和使用高分辨率质谱反应方案进行精确质量测量后,可以为所有研究的β-内酰胺类抗生素提出反应方案。主要反应是β-内酰胺环的水解,生成哌啶取代的酰胺。对于一些β-内酰胺类抗生素,根据预期得到了多种等质量的水解反应产物,但这并不妨碍定量分析。最终方法完全按照委员会决议 2002/657/EC 进行了定量确证残留分析方法验证,除比阿培南外,所有化合物的准确度在 80%至 110%之间,目标水平下的实验室内重复性低于 22%,均表现出满意的定量性能。对于比阿培南,该方法仅被证明适用于定性分析。

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