Development and validation of a multiclass method for the determination of antibiotic residues in honey using liquid chromatography-tandem mass spectrometry.
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-1and from 7 to 13 µg kg-1, respectively, except for streptomycin and neomycin, which showed slightly higher CCα at 25 µg kg-1and 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.
a CNRSL, Lebanese Atomic Energy Commission (LAEC) , Laboratory for Analysis of Organic Compound (LAOC) , Beirut , Lebanon.|c French Agency for Safety of Food, Environment and Occupational Health , Laboratory of Fougères, French National and European Union Reference Laboratory for Residues of Antimicrobial Veterinary Medicinal Products in Food from Animal Origin , Fougères , France.
Khaled
K
El Hawari
a CNRSL, Lebanese Atomic Energy Commission (LAEC) , Laboratory for Analysis of Organic Compound (LAOC) , Beirut , Lebanon.
Samia
S
Mokh
b Faculty of Public Health I , Lebanese University , Hadath, Beirut , Lebanon.
Samah
S
Doumyati
a CNRSL, Lebanese Atomic Energy Commission (LAEC) , Laboratory for Analysis of Organic Compound (LAOC) , Beirut , Lebanon.|b Faculty of Public Health I , Lebanese University , Hadath, Beirut , Lebanon.
Mohamad
M
Al Iskandarani
c French Agency for Safety of Food, Environment and Occupational Health , Laboratory of Fougères, French National and European Union Reference Laboratory for Residues of Antimicrobial Veterinary Medicinal Products in Food from Animal Origin , Fougères , France.
Eric
E
Verdon
D000617:Aminoglycosides / Q000032:analysis; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D001516:Bees / Q000502:physiology; D002853:Chromatography, Liquid / Q000592:standards*; D004335:Drug and Narcotic Control / Q000331:legislation & jurisprudence; D005062:European Union; D005506:Food Contamination / Q000032:analysis*; D006722:Honey / Q000032:analysis*; D006801:Humans; D055231:Lincosamides / Q000032:analysis; D018942:Macrolides / Q000032:analysis; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods; D013449:Sulfonamides / Q000032:analysis; D053719:Tandem Mass Spectrometry / Q000592:standards*; D013754:Tetracyclines / Q000032:analysis; D019155:Veterinary Drugs / Q000032:analysis*
D000617:Aminoglycosides; D000900:Anti-Bacterial Agents; D055231:Lincosamides; D018942:Macrolides; D013449:Sulfonamides; D013754:Tetracyclines; D019155:Veterinary Drugs
LC-MS/MS; Multi-class analysis; honey; validation; veterinary drugs