Multiclass Analysis of Antibiotic Residues in Honey by Ultraperformance Liquid Chromatography−Tandem Mass Spectrometry

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• 作者：Jose Luis Martnez Vidal ; Mara del Mar Aguilera-Luiz ; Roberto Romero-Gonzlez ; Antonia Garrido Frenich*
• 刊名：Journal of Agricultural and Food Chemistry
• 出版年：2009
• 出版时间：March 11, 2009
• 年：2009
• 卷：57
• 期：5
• 页码：1760-1767
• 全文大小：195K
• 年卷期：v.57,no.5(March 11, 2009)
• ISSN：1520-5118

文摘

A method has been developed and validated for the simultaneous analysis of different veterinary drug residues (macrolides, tetracyclines, quinolones, and sulfonamides) in honey. Honey samples were dissolved with Na₂EDTA, and veterinary residues were extracted from the supernatant by solid-phase extraction (SPE), using OASIS HLB cartridges. The separation and determination was carried out by ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS), using an electrospay ionization source (ESI) in positive mode. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring (MRM) of two ion transitions per compound to provide a high degree of sensitivity and specificity. The method was validated, and mean recoveries were evaluated at three concentration levels (10, 50, and 100 μg/kg), ranging from 70 to 120% except for doxycycline, erythromycin, and tylmicosin with recovery higher than 50% at the three levels assayed. Relative standard deviations (RSDs) of the recoveries were less than 20% within the intraday precision and less than 25% within the interday precision. The limits of quantification (LOQs) were always lower than 4 μg/kg. The developed procedure was applied to 16 honey samples, and erythromycin, sarafloxacin, and tylosin were found in a few samples.