Comprehensive screening and quantification of veterinary drugs in milk using UPLC-ToF-MS
| Autor: | M.W.F. Nielen, J. Efraim Oosterink, A.A.M. Stolker, J.J.P. Lasaroms, J.A. van Rhijn, Ruud J. B. Peters, P. Rutgers |
|---|---|
| Jazyk: | angličtina |
| Rok vydání: | 2008 |
| Předmět: |
Veterinary Drugs
muscle residue analysis Multi-residue Solid-phase microextraction Tandem mass spectrometry Biochemistry Multi-class Analytical Chemistry Tandem Mass Spectrometry Validation Protein precipitation Animals Chemical Precipitation Solid phase extraction Full scan growth-promoting agents Chromatography High Pressure Liquid Solid Phase Microextraction 2002/657/EC BU Microbiological & Chemical Food Analysis Original Paper Chromatography Chemistry Time-of-flight Organic Chemistry Repeatability Raw milk Organische Chemie urine Milk flight mass-spectrometry strategies BU Microbiologische & Chemische Voedselanalyse Quantitative analysis (chemistry) |
| Zdroj: | Analytical and Bioanalytical Chemistry 391 (2008) 6 Analytical and Bioanalytical Chemistry, 391(6), 2309-2322 Analytical and Bioanalytical Chemistry |
| ISSN: | 1618-2642 |
| Popis: | Ultra-performance liquid chromatography combined with time-of-flight mass spectrometry (UPLC-ToF-MS) has been used for screening and quantification of more than 100 veterinary drugs in milk. The veterinary drugs represent different classes including benzimidazoles, macrolides, penicillins, quinolones, sulphonamides, pyrimidines, tetracylines, nitroimidazoles, tranquillizers, ionophores, amphenicols and non-steroidal anti-inflammatory agents (NSAIDs). After protein precipitation, centrifugation and solid-phase extraction (SPE), the extracts were analysed by UPLC-ToF-MS. From the acquired full scan data the drug-specific ions were extracted for construction of the chromatograms and evaluation of the results. The analytical method was validated according to the EU guidelines (2002/657/EC) for a quantitative screening method. At the concentration level of interest (MRL level) the results for repeatability (%RSD20% for 86% of the compounds), reproducibility (%RSD40% for 96% of the compounds) and the accuracy (80-120% for 88% of the compounds) were satisfactory. Evaluation of the CCbeta values and the linearity results demonstrates that the developed method shows adequate sensitivity and linearity to provide quantitative results. Furthermore, the method is accurate enough to differentiate between suspected and negative samples or drug concentrations below or above the MRL. A set of 100 samples of raw milk were screened for residues. No suspected (positive) results were obtained except for the included blind reference sample containing sulphamethazine (88 microg/l) that tested positive for this compound. UPLC-ToF-MS combines high resolution for both LC and MS with high mass accuracy which is very powerful for the multi-compound analysis of veterinary drugs. The technique seems to be powerful enough for the analysis of not only veterinary drugs but also organic contaminants like pesticides, mycotoxins and plant toxins in one single method. |
| Databáze: | OpenAIRE |
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