Confirmatory method for the determination of nitroimidazoles in milk by liquid chromatography - tandem mass spectrometry

• Autorzy: Mitrowska K. , Antczak M. , Posyniak A.
• Języki publikacji: EN

Abstrakty

EN

A multiresidue method for the determination of seven nitroimidazoles and their hydroxy metabolites in milk was developed. Milk samples were extracted with acetonitrile and cleaned up on strong cation-exchange solid phase extraction cartridges. Evaporated to dryness first, the extracts obtained were then reconstituted in 0.1% formic acid and injected onto a liquid chromatography-tandem mass spectrometer (LC-MS/MS). The separation of analytes was achieved on gradient mode using a C18 column and a mobile phase consisting of 0.1% formic acid in acetonitrile and 0.1% formic acid in water. Multiple reaction monitoring mode was set for the MS/MS with positive electrospray ionisation. For quantification, the isotope dilution method was used with isotopicalh labeled analogues of the target analytes. The method was evaluated entirely in accordance with EU Commission Decision 2002/657/EC and all validation criteria were in the required ranges. The method can easily detect and confirm metronidazole, dimetridazole, ronidazole, ipronidazole, and their hydroxy metabolites below the recommended concentration level of 3 µg/kg. The decision limits and detection capabilities ranged from 0.11 µg/kg to 0.22 µg/kg and from 0.19 µg/kg to 0.37 µg/kg respectively. The overall recoveries were between 96.6% and 105.2% with a good coefficient of variation, less than 8.7% under within-laboratory reproducibility conditions.

• Wydawca: -
• Czasopismo: Bulletin of the Veterinary Institute in Puławy
• Rocznik: 2014
• Tom: 58
• Numer: 4
• Opis fizyczny: p.581-587,fig.,ref.

Twórcy

autor

Mitrowska K.

• Department of Pharmacology and Toxicology, National Veterinary Research Institute, 24-100 Pulawy, Poland

autor

Antczak M.

• Department of Pharmacology and Toxicology, National Veterinary Research Institute, 24-100 Pulawy, Poland

autor

Posyniak A.

• Department of Pharmacology and Toxicology, National Veterinary Research Institute, 24-100 Pulawy, Poland

Bibliografia

• 1. Commission Decision 2002/657/EC. Off J Eur Commun 2002, L221, 8-36.
• 2. Commission Regulation EU No 37/2010. Off J Eur Commun 2010, L15, 1-72.
• 3. Council Directive 96/23/EC. Off J Eur Commun 1996, L125, 10-32.
• 4. CRL Guidance Paper, CRLs view on state of the art analytical methods for national residue control plans. 2007, December 2007.
• 5. Cronly M., Behan P., Foley B., Malone E., Martin S., Doyle M., Regan L.:. Rapid multi-class multi-residue method for the confirmation of chloramphenicol and eleven nitroimidazoles in milk and honey by liquid chromatography-tandem mass spectrometry (LC-MS). Food Addit Contam Part A 2010, 27, 1233-1246.
• 6. European Commission: Commission Decision 2002/657/EC. Off J Eur Commun 2002, L 221, 8-36.
• 7. Hernandez-Mesa M., Garcia-Campana A.M., Cruces- Blanco C.: Novel solid phase extraction method for the analysis of 5-nitroimidazoles and metabolites in milk samples by capillary electrophoresis. Food Chem 2014, 145, 161-167.
• 8. International Agency for Research on Cancer (IARC): Monographs on the evaluation of carcinogenic risks to humans. Overall evaluations of carcinogenicity. Supplement 7 1987, 250.
• 9. Mitrowska K., Posyniak A., Zmudzki J.: Multiresidue method for the determination of nitroimidazoles and their hydroxv- metabolites in poultry muscle, plasma and egg by isotope dilution liquid chromatography mass spectrometry. Talanta 2010, 81, 1273-1280.
• 10. Ortelli D., Cognard E., Jan P., Edder P.: Comprehensive fast multiresidue screening of 150 veterinary drugs in milk by ultra- performance liquid chromatography coupled to time of flight mass spectrometry. J Chromatogr B 2009, 877, 2363-2374.
• 11. Robert C., Gillard N., Brasseur P.Y., Pierret G., Ralet N., Dubois M., Delahaut P.: Rapid multi-residue and multi-class qualitative screening for veterinary drugs in foods of animal origin by UHPLC-MS/MS. Food Add Contamin Part A - Chem Anal Control Exposure Risk Assess 2013, 30, 443-457.
• 12. Stolker A.A., Rutgers P., Oosterink E., Lasaroms J.J., Peters R.J., van Rhijn J.A., Nielen M.W.: Comprehensive screening and quantification of veterinary drugs in milk using UPLC-ToF-MS. Anal Bioanal Chem 2008, 391, 2309-2322.
• 13. Thompson C.S., Traynor I.M., Fodey T.L., Crooks S.R.: Improved screening method for the detection of a range of nitroimidazoles in various matrices by optical biosensor. Anal Chim Acta 2009, 637, 259-264.
• 14. Tolgyesi A., Sharma V.K., Fekete S., Fekete J., Simon A., Farkas S.: Development of a rapid method for the determination and confirmation of nitroimidazoles in six matrices by fast liquid chromatography-tandem mass spectrometry. J Pharm Biomed Anal 2012, 64-65, 40-48.