Development of a multi-class method for the quantification of veterinary drug residues in feedingstuffs by liquid chromatography-tandem mass spectrometry

• Published in: Journal of Chromatography A Vol. 1217; no. 41; pp. 6394 - 6404
• Main Authors: Boscher, Aurore, Guignard, Cédric, Pellet, Terence, Hoffmann, Lucien, Bohn, Torsten
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 08-10-2010; Amsterdam; New York: Elsevier; Elsevier
• Subjects: Analysis of Variance; Animal Feed - analysis; Anti-Bacterial Agents - analysis; Antibiotics; Biological and medical sciences; Chromatography, Liquid - methods; Coccidiostats; Drug Residues - analysis; Feed; Feed and pet food industries; Food industries; Fundamental and applied biological sciences. Psychology; LC–MS/MS; Linear Models; Matrix effects; Reproducibility of Results; Sensitivity and Specificity; Solid Phase Extraction; Standard addition method; Tandem Mass Spectrometry - methods; Temperature; Veterinary Drugs - analysis; Matrix effects; Coccidiostats; Standard addition method; Antibiotics; LC–MS/MS; Feed; Solid phase extraction; Tandem mass spectrometry; Chemical analysis; HPLC chromatography; Solvent extraction; Veterinary medicine; Electrospray; Chemical enrichment; Antiprotozoal agent; LC-MS/MS; Dispersive Solid-Phase Extraction; Ultrasound assisted extraction; Sample preparation; Ultrasound; Ungulata; Quantitative analysis; Validation; Coupled method; Matrix effect; Contamination; Operating conditions; Pig; Vertebrata; Antibiotic; Mammalia; Multicomponent analysis; Pressure effect; Residue; Parasiticide; Artiodactyla; Antibacterial agent
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2010.08.024

A simple multi-residue method was developed for detecting and quantifying 33 analytes from 13 classes of antibiotics (tetracyclines (3), quinolones (7), penicillins (3), ionophore coccidiostats (7), macrolides (3), sulfonamides (1), quinoxalines (2), phenicols (2), lincosamides (1), diaminopyrimidines (1), polypeptides (1), streptogramins (1) and pleuromutilins (1)) in animal feeds. Extraction and clean-up procedures were optimized with spiked piglet feed. Samples were extracted by ultrasonic-assisted extraction with a mixture of methanol/acetonitrile/McIlvaine buffer at pH 4.6 (37.5/37.5/25, v/v/v) containing 0.3% of EDTA-Na
2, followed by a clean up using a dispersive solid-phase extraction (d-SPE) with PSA (primary secondary amine). Detection of antibiotics was achieved by liquid chromatography-electrospray tandem mass spectrometry (LC–ESI-MS/MS) within 28
min using both positive and negative ESI mode. Average recoveries ranged from 51% (oxytetracycline) to 116% (tilmicosin) with associated relative standard deviations of 7.3% and 9.0% and an overall mean of 87%. Limits of quantification ranged from 3.8
ng
g
−1 (lincomycin) to 65.0
ng
g
−1 (bacitracin). Following optimization, the method was further verified for bovine and lamb feedingstuffs; negative matrix effects were evaluated and overcome by a standard addition method.