Development of a rapid method for the analysis of synthetic growth promoters in bovine muscle using liquid chromatography tandem mass spectrometry
| Autor: | Liam Regan, D.G. Kennedy, Christopher T. Elliott, Edward Malone |
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| Rok vydání: | 2009 |
| Předmět: |
Spectrometry
Mass Electrospray Ionization Electrospray ionization Tandem mass spectrometry Mass spectrometry Sensitivity and Specificity Biochemistry Analytical Chemistry Melengestrol acetate chemistry.chemical_compound Anabolic Agents Tandem Mass Spectrometry Liquid chromatography–mass spectrometry medicine Animals Environmental Chemistry Solid phase extraction Chromatography High Pressure Liquid Spectroscopy Chromatography Chemistry Muscles Solid Phase Extraction Dienestrol Reproducibility of Results Drug Residues Substance Abuse Detection Hexestrol Cattle medicine.drug |
| Zdroj: | Analytica Chimica Acta. 637:112-120 |
| ISSN: | 0003-2670 |
| DOI: | 10.1016/j.aca.2008.09.002 |
| Popis: | A rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous identification, confirmation and quantitation of thirteen synthetic growth promoters in bovine muscle. The method was validated in accordance with the criteria defined in Commission Decision 2002/657/EC. A value of 1mugkg(-1) was chosen as the required performance level (RPL) for all analytes. The growth promoters investigated were alpha and beta trenbolone, 16-beta-OH stanozolol, methylboldenone, fluoxymesterone, methyltestosterone, medroxyprogesterone acetate, megestrol acetate, melengestrol acetate, dexamethasone, flumethasone, dienestrol and hexestrol. The method involved enzymatic hydrolysis, purification by solid phase extraction followed by analysis by UPLC-MS/MS using electrospray ionization operated in both positive and negative polarities with a total run time of 14 min. The decision limit (CCalpha) values obtained, ranged from 0.09 to 0.19 microgkg(-1) and the detection capability (CCbeta) values obtained, ranged from 0.15 to 0.32 microgkg(-1). The results of the inter-assay study, which was performed by fortifying bovine muscle samples (n=18) on three separate days, show the accuracy calculated for the various analytes to range between 98% and 102%. The precision of the method, expressed as R.S.D. values for the inter-assay variation of each analyte at the three levels of fortification (1, 1.5 and 2.0 microgkg(-1)), ranged between 3.1% and 5.8%. A Day 4 assay was carried out to examine variations due to different animals and different muscle types. |
| Databáze: | OpenAIRE |
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