Development and validation of a multiclass method for the determination of antibiotic residues in honey using liquid chromatography-tandem mass spectrometry

Abstract : A new, simple and fast method was developed for the determination of multi-class antibiotic residues in honey (sulfonamides, tetracyclines, macrolides, lincosamides and aminoglycosides). Separation and determination were carried out by LC-MS/MS. During sample preparation, various parameters affecting extraction efficiency were examined, including the type of solvent, pH, efficiencies of cleavage of N-glycosidic linkages by hydrochloric acid, ultrasonic extraction and its duration compared with shaking, along with dispersive SPE clean-up. Experiments with fortified samples demonstrated that 10 min of ultrasonic treatment with acidified methanol (HCl 2 M) followed by dispersive SPE clean-up with 50 mg PSA gave an effective sample preparation method for several classes of antibiotics in honey. Anhydroerythromycin A, erythromycin A enol ether and desmycosin were used as markers for the presence of erythromycin A and tylosin A in honey samples. The method was validated according to European Commission Decision (EC) No. 2002/657. The recoveries of analytes ranged from 85% to 111%. Repeatability and intra-laboratory reproducibility were < 20.6% and 26.8%, respectively. Decision limit (CCα) and detection capability (CCβ) ranged from 6 to 9 µg kg– 1 and from 7 to 13 µg kg– 1, respectively, except for streptomycin and neomycin, which showed slightly higher CCα at 25 µg kg– 1 and CCβ at 34 µg kg– 1. Finally, the method was applied to the honey test material 02270 through a FAPAS proficiency test (PT) for the determination of tetracyclines. PT results were obtained within a z-score range of ±2, proving that the validated method is suitable for routine analysis to ensure the quality of honey.
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Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment, 2017, 34 (4), pp.582-597. 〈http://www.tandfonline.com/doi/full/10.1080/19440049.2016.1232491〉. 〈10.1080/19440049.2016.1232491〉
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Soumis le : lundi 19 décembre 2016 - 14:23:26
Dernière modification le : mardi 9 janvier 2018 - 01:00:53

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Khaled El Hawari, S Mokh, S Doumyati, M Al Iskandarani, Eric Verdon. Development and validation of a multiclass method for the determination of antibiotic residues in honey using liquid chromatography-tandem mass spectrometry. Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment, 2017, 34 (4), pp.582-597. 〈http://www.tandfonline.com/doi/full/10.1080/19440049.2016.1232491〉. 〈10.1080/19440049.2016.1232491〉. 〈anses-01419435〉

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