Validation of a method for the determination of aminoglycosides in different matrices and species based on an in-house concept

• Published in: Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment Vol. 30; no. 6; pp. 1037 - 1043
• Main Authors: Bohm, D.A, Stachel, C.S, Gowik, P
• Format: Journal Article Conference Proceeding
• Language: English
• Published: Abingdon Taylor & Francis 01.06.2013
• Subjects: Aminoglycosides - analysis; antibiotics; apramycin; Biological and medical sciences; Chromatography, Liquid; clean-up; dihydrostreptomycin; extraction; Food industries; Fundamental and applied biological sciences. Psychology; gentamicin; kidneys; LC-MS/MS; maximum residue limits; method validation; milk; neomycin; Solid Phase Extraction; spectinomycin; swine; Tandem Mass Spectrometry - methods; tissue and milk; tobramycin; trichloroacetic acid; veterinary drug residues; Drug; Validation; method validation; clean-up; Dairy product; Liquid chromatography; Method; tissue and milk; veterinary drug residues; Tissue; LC-MS/MS; Antibiotic; Residue; Extraction; Species; antibiotics; Milk
• ISSN: 1944-0057; 1944-0049; 1944-0057
• DOI: 10.1080/19440049.2013.775709

A simple, rapid, and sensitive method for the determination and confirmation of the aminoglycosides streptomycin, dihydrostreptomycin, spectinomycin, apramycin, kanamycin, paromomycin, gentamicin and neomycin in cow’s milk as well as in bovine and porcine muscle and kidney was developed. Validation was performed on the basis of an in-house concept with different factor-level combinations in accordance with Commission Decision 2002/657/EC. After extraction with trichloroacetic acid solution, clean-up was performed by way of SPE. LC-MS/MS analysis was carried out by means of an HILIC column for the separation of the analytes, and by using MS/MS in positive ESI mode to measure the transitions of the substances in MRM mode. For quantification, matrix calibration curves in the linear range around the MRLs as well as the internal standard tobramycin were used. The calculated validation parameters like CCα, CCβ, recovery (94–103%), relative repeatability RSDᵣ (3.6–9.7%), and relative within-laboratory reproducibility RSDwR (4.6–10.0%) fulfilled the requirements of Commission Decision 2002/657/EC.