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超高效液相色谱串联质谱法测定牛肌肉中抗生素的多残留多类别方法

Multi-residue and multi-class method for the determination of antibiotics in bovine muscle by ultra-high-performance liquid chromatography tandem mass spectrometry.

作者信息

Freitas Andreia, Barbosa Jorge, Ramos Fernando

机构信息

INIAV-LNIV, Laboratório Nacional de Investigação Veterinária, Estrada de Benfica, 701, 1549-011 Lisboa, Portugal.

CNC - Centro de Neurociências e Biologia Celular, Pólo das Ciências da Saúde, Faculdade de Farmácia, Universidade de Coimbra, Azinhaga de Santa Comba, 3000-548 Coimbra, Portugal.

出版信息

Meat Sci. 2014 Sep;98(1):58-64. doi: 10.1016/j.meatsci.2014.04.003. Epub 2014 Apr 18.

Abstract

A multi-residue quantitative screening method covering 41 antibiotics from 7 different families, by ultra-high-performance-liquid-chromatography tandem mass spectrometry (UHPLC-MS/MS), is described. Sulfonamides, trimethoprim, tetracyclines, macrolides, quinolones, penicillins and chloramphenicol are simultaneously detected after a simple sample preparation of bovine muscle optimized to achieve the best recovery for all compounds. A simple sample treatment was developed consisting in an extraction with a mixture of acetonitrile and ethylenediaminetetraacetic acid (EDTA), followed by a defatting step with n-hexane. The methodology was validated, in accordance with Decision 2002/657/EC by evaluating the required parameters: decision limit (CCα), detection capability (CCβ), specificity, repeatability and reproducibility. Precision in terms of relative standard deviation was under 20% for all compounds and the recoveries between 91% and 119%. CCα and CCβ were determined according the maximum residue limit (MRL) or the minimum required performance limit (MRPL), when required.

摘要

本文描述了一种采用超高效液相色谱串联质谱法(UHPLC-MS/MS)对来自7个不同家族的41种抗生素进行多残留定量筛查的方法。在对牛肌肉样本进行简单预处理以实现所有化合物的最佳回收率后,可同时检测磺胺类药物、甲氧苄啶、四环素、大环内酯类、喹诺酮类、青霉素类和氯霉素。开发了一种简单的样品处理方法,先用乙腈和乙二胺四乙酸(EDTA)混合物进行萃取,然后用正己烷进行脱脂步骤。该方法根据2002/657/EC号决定进行了验证,通过评估所需参数:决策限(CCα)、检测能力(CCβ)、特异性、重复性和再现性。所有化合物的相对标准偏差精度均低于20%,回收率在91%至119%之间。必要时,根据最大残留限量(MRL)或最低所需性能限量(MRPL)确定CCα和CCβ。

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