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Title: Rapid multi-residue LC-MS/MS determination of nitrofuran metabolites, nitroimidazoles, amphenicols, and quinolones in honey with ultrasonic-assisted derivatization - magnetic solid-phase extraction. Author: Melekhin AO, Tolmacheva VV, Goncharov NO, Apyari VV, Parfenov MY, Bulkatov DP, Dmitrienko SG, Zolotov YA. Journal: J Pharm Biomed Anal; 2024 Jan 05; 237():115764. PubMed ID: 37804641. Abstract: A rapid multi-residue LC-MS/MS method for the identification and determination of banned veterinary drugs in honey was developed. A total of 31 investigated veterinary drugs belonging to 4 classes including nitrofurans metabolites, nitroimidazoles, amphenicols, and quinolones were quantified by LC-MS/MS with ESI using one single injection. The sample preparation included treatment with 5-nitro-2-furaldehyde (5-NFA) in a thermostated ultrasonic bath (80 °C, 0.5М НСl, 20 min) to liberate matrix-bound residues of nitrofurans. Magnetic hypercrosslinked polystyrene (HCP/Fe3O4) was proposed for the solid-phase extraction and clean-up of target analytes prior to LC-MS/MS analysis. To evaluate and validate the performance of method, the criteria of the Decision (EC) no 2002/657 were applied. The LOQs of the examined analytes range from 0.3 to 1 μg kg-1, which indicates good sensitivity to quantify the target compounds in honey. The recoveries of veterinary drugs from 1 g of honey with 50 mg of the sorbent are 97-109% for nitrofuran metabolites, 84-115% for nitroimidazoles, 86-103% for amphenicols, and 97-118% for quinolones. The relative standard deviations of intra-day and inter-day precision analyses (RSD) are less than 16%. This methodology was applied to real honey samples and trace levels of some veterinary drugs were detected.[Abstract] [Full Text] [Related] [New Search]