Determination of levamisole in feeds by liquid chromatography coupled to electrospray mass spectrometry on an ion trap |
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Authors: | Gallo Pasquale Fabbrocino Serena Serpe Luigi |
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Institution: | Dept. of Chemistry, Istituto Zooprofilattico Sperimentale del Mezzogiorno, via Salute 2, Portici, NA 80055, Italy. pasquale.gallo@cert.izsmportici.it |
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Abstract: | Test methods have to be developed by laboratories for official control to monitor possible misuse of veterinary drugs in animal productions, also through feeding stuff. A novel method for identification and quantification of levamisole in feeds by liquid chromatography coupled to electrospray mass spectrometry in an ion trap (LC/ESI-MS/MS) is herein described; after a single-step cleanup by liquid-liquid extraction from the feed and separation by reversed-phase liquid chromatography, levamisole was determined and unambiguously confirmed by tandem mass spectrometry, on the basis of two product ions. The method was in-house validated, according to the Regulation 882/2004/EC, evaluating trueness, repeatability, within-laboratory reproducibility, ruggedness, specificity, and the limit of quantification (LOQ). The method is reliable and specific for complete and complementary feeds for pigs, cattle, rabbits and poultry; very good mean recoveries (higher than 92 %) and precision (RSD values?15.2%) were attained. The LOQ at 2.0?mg/kg was verified. Moreover, we describe how the method was developed to support Italian Police investigations regarding illegal treatments of pigs; in this case, since the drug(s) added to the feed were unknown, a preliminary untargeted analysis was performed by full scan mass spectrometry on an ion trap, from 50 up to 2000?m/z; the presence of levamisole was hypothesised, on the basis of the most abundant ion and its fragmentation pattern. Then, levamisole was unambiguously confirmed by the ion trap LC/ESI-MS/MS method. |
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