Development and validation of a modified QuEChERS protocol coupled to LC–MS/MS for simultaneous determination of multi-class antibiotic residues in honey

• Published in: Food chemistry 2016-01, Vol.190, p.982-989
• Main Authors: Shendy, Amr H., Al-Ghobashy, Medhat A., Gad Alla, Sohair A., Lotfy, Hayam M.
• Format: Article
• Language: English
• Subjects: AHD; AMOZ; Anti-Bacterial Agents - analysis; Anti-Bacterial Agents - isolation & purification; AOZ; Calibration; Chromatography, Liquid - methods; Dimetridazole; Drug Residues - analysis; Drug Residues - isolation & purification; Honey; Honey - analysis; LC–MS/MS; Nitrofuran; Nitroimidazoles; Ronidazole; SEM; Tandem Mass Spectrometry - methods; Veterinary drug residues
• ISSN: 0308-8146; 1873-7072
• DOI: 10.1016/j.foodchem.2015.06.048

•LC–MS/MS assay was developed and validated for determination of nitrofuran metabolites and nitroimidazole residues in honey.•Derivatisation of nitrofuran metabolites and a modified QuEChERS protocol were successfully employed.•The use of neat standard calibration curves in conjunction with a correction factor for matrix effect is presented. LC–MS/MS assay was developed and validated according to EU guidelines for determination of nitrofuran metabolites and nitroimidazole residues in honey. Crude samples were acid-treated to liberate matrix-bound residues and a modified QuEChERS protocol was employed. Nitrofurantoin, furazolidone, furaltadone and nitrofurazone were determined via analysis of their metabolites AHD, AOZ, AMOZ and SEM, respectively while nitroimidazole residues; ronidazole (RNZ) and dimetridazole (DMZ) were determined directly. For all analytes, neat standard calibration curves, after correction for matrix effect were successfully employed. Decision limit (CCα) and detection capability (CCβ) were below the MRPL for nitrofurans (1.00μgkg−1) and the recommended concentration for nitroimidazole (3.00μgkg−1), respectively. The CCα, CCβ, percentage recovery and CV% ranges were 0.12–0.74μgkg−1, 0.21–1.27μgkg−1, 90.96–104.80% and 2.65–12.58%, respectively. This work is part of the national initiative for establishing a national monitoring program for drug residues in Egyptian honey.