Comprehensive screening and quantification of veterinary drugs in milk using UPLC–ToF-MS

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 (%RSD < 20% for 86% of the compounds), reproducibility (%RSD < 40% for 96% of the compounds) and the accuracy (80–120% for 88% of the compounds) were satisfactory. Evaluation of the CCβ 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 μg/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

Correlation between non-reversible thallium-201 myocardial perfusion defect and ECG criteria in the diagnosis of apical myocardial infarction

Background: ECG identification of apical myocardial infarction (MI) is controversial and lacks of accuracy. Our aim was to investigate the sensitivity of different proposed ECG criteria in the presence of apical perfusion defects assessed with SPECT analysis. Methods: One hundred twenty-four (98 M, 26 F) out of 1500 patients with suspected coronary artery disease, showed apical perfusion defect not reversible at rest and after reinjection at tomographic SPECT analysis during thallium-201 scintigraphy. Results: In the group of 29 patients presenting wide isolated apical perfusion defect (wAPD) Q waves in anterior segments with definition of antero-septal MI was prevalent (51.7%), while few patients (41.3%) presented the ECG criteria of apical MI as proposed in the literature. In 19 of the 25 patients with partial isolated apical perfusion defect (pAPD), the absence of Q wave was clearly prevalent. Fifty patients had a wAPD partially extended in surrounding regions, as anterior or septal, inferior or lateral myocardial segments, in these patients, the site of Q wave location was more variable, with prevalent Q wave in anterior leads, but with more incidence of Q waves in leads II III aVF, especially in patients with associated perfusion defect in inferior segments. Substantially, the same finding resulted in the 20 patients showing a pAPD extended in surrounding myocardial segments. Conclusion: In conclusion, the low diagnostic sensitivity of the ECG criteria of identification of apical MI is clearly demonstrated by our analysis carried out using SPECT perfusion scintigraphy, with ECG findings of anterior/anterior- septal myocardial necrosis in the patients with wAPD