Multiresidue method for the determination of nitroimidazoles and their hydroxy-metabolites in poultry muscle, plasma and egg by isotope dilution liquid chromatography–mass spectrometry

• Published in: Talanta (Oxford) 2010-06, Vol.81 (4), p.1273-1280
• Main Authors: Mitrowska, Kamila, Posyniak, Andrzej, Zmudzki, Jan
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Animals; Calibration; Chemistry; Chemistry Techniques, Analytical; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid - methods; Eggs - analysis; Exact sciences and technology; Food Analysis; Isotope dilution; Limit of Detection; Liquid chromatography; Mass spectrometry; Mass Spectrometry - methods; Metabolites; Muscle, Skeletal - drug effects; Muscle, Skeletal - metabolism; Nitroimidazoles; Nitroimidazoles - analysis; Nitroimidazoles - chemistry; Other chromatographic methods; Poultry; Reproducibility of Results; Residues; Spectrometric and optical methods; Time Factors
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2010.02.020

A multiresidue analytical procedure for the determination of four nitroimidazoles (metronidazole, dimetridazole, ronidazole, ipronidazole) and their hydroxy-metabolites in poultry muscle, plasma and egg is presented. The procedure is based on ion-exchange solid phase extraction with acetonitrile as an extractant followed by liquid chromatography–mass spectrometry. The separation of analytes was performed on a C18 column using a mobile phase of 0.1% formic acid in acetonitrile and 0.1% formic acid in water with gradient elution. The electrospray ionization was used to obtain the protonated molecules [M+H] + and two product ions were monitored for each compound. For the quantification stable isotope-labelled analogues of the analytes were used as internal standards. The whole procedure was evaluated according to EU Commission Decision 2002/657/EC requirements. Specificity, decision limit (CCα), detection capacity (CCβ), recovery and precision were determined during validation process. The overall recoveries ranged between 93 and 103% with a good coefficient of variation, less than 14.0% under within-laboratory reproducibility conditions. CCα and CCβ were 0.05–0.44 and 0.08–0.90 μg kg −1 depending on analyte and matrix.