Determination of levamisole in feeds by liquid chromatography coupled to electrospray mass spectrometry on an ion trap.

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).

Confirmatory analysis of non-steroidal anti-inflammatory drugs in bovine milk by high-performance liquid chromatography with fluorescence detection.

HPLC with fluorescence detection is considered for confirmatory analysis of group B veterinary drugs by the European Union legislation. A procedure for confirming the presence of anti-inflammatory non-steroidal drug (NSAID) residues in bovine milk by reversed phase high-performance liquid chromatography with fluorescence detection is herein described. The native fluorescence of nine drugs belonging to different NSAID sub-classes, namely flurbiprofen, carprofen, naproxen, vedaprofen, 5-hydroxy-flunixin, niflumic acid, mefenamic acid, meclofenamic acid and tolfenamic acid, allowed for detection in bovine milk down to 0.

Determination of the banned growth promoter moenomycin A in feed stuffs by liquid chromatography coupled to electrospray ion trap mass spectrometry.

Flavomycin complex is an antibiotic banned in the European Union as an additive in feed stuffs. As a consequence, the monitoring programmes for official control within the Community require analysis of feeds for possible illegal use of flavomycin. A method for unambiguous identification and quantification of moenomycin A, the main pharmacologically active component of flamomycin complex, in several feeds by liquid chromatography coupled to electrospray ion trap mass spectrometry (LC/ESI-MS/MS) is herein described for the first time.

Determination of cylindrospermopsin in freshwaters and fish tissue by liquid chromatography coupled to electrospray ion trap mass spectrometry.

Cylindrospermopsin (CYN) is a toxic alkaloid-like compound produced by some strains of cyanobacteria, procariotic organisms occurring in water blooms, observed worldwide in eutrophic lakes and drinking water reservoirs. Methods for determination of CYN in freshwater and fish muscle by liquid chromatography coupled to electrospray ion trap mass spectrometry are herein described. The performances of both methods are reported; ion trap LC/ESI-MS/MS resulted highly selective and reliable in unambiguous identification of CYN, based on monitoring the precursor ion and three product ions.

Characterisation of biotoxins produced by a cyanobacteria bloom in Lake Averno using two LC-MS-based techniques.

Cyanobacteria (blue-green algae) cause blooms in eutrophic lakes and drinking water reservoirs. They also produce biotoxins, including microcystins (MCs), highly toxic cyclic heptapeptides that cause poisoning in animals and human. In this paper, we present a method for the analysis of four MCs by ion trap LC-MS and MALDI-TOF/MS.

Liquid chromatography coupled to quadruple time-of-flight tandem mass spectrometry for microcystin analysis in freshwaters: method performances and characterisation of a novel variant of microcystin-RR.

Cyanobacteria, also called blue-green algae, occur worldwide within water blooms in eutrophic lakes and drinking water reservoirs, producing several biotoxins (cyanotoxins). Among these, microcystins (MCs) are a group of cyclic heptapeptides showing potent hepatotoxicity and activity as tumour promoters. So far, at least 89 MCs from different cyanobacteria genera have been characterised.

Confirmatory identification of sixteen non-steroidal anti-inflammatory drug residues in raw milk by liquid chromatography coupled with ion trap mass spectrometry.

The European Council Decision 2002/657/EC established that group B substances detected in foods must be identified and confirmed on the basis of their molecular structure. To this aim, we have developed a panel of methods for unambiguous determination of sixteen non-steroidal anti-inflammatory drugs (NSAIDs) in cattle and buffalo raw milk. A multi-residue reversed-phase high-performance liquid chromatography method with photodiode array detection is described for quantitative screening analysis.

Multi-residue determination of non-steroidal anti-inflammatory drug residues in animal serum and plasma by HPLC and photo-diode array detection.

The European Union regulated the use of non-steroidal anti-inflammatory drugs (NSAIDs) in animal production and set the official analytical controls to detect their residues in plasma, serum, and milk within the frame of national monitoring programs in each member state. In this work, a multi-residue reversed-phase high-performance liquid chromatography with diode array detector (DAD) method is described for the simultaneous determination of 13 NSAIDs in serum and plasma of farm animals. Chromatographic separation by a C12 stationary phase column with a linear gradient is able to resolve all the compounds considered: salicylic acid, ketoprofen, flurbiprofen, phenylbutazone and its metabolite (oxyphenbutazone), carprofen, ibuprofen, naproxen, niflumic acid, suxibutazone, diclofenac, mefenamic acid, and tolfenamic acid.

Determination of fourteen non-steroidal anti-inflammatory drugs in animal serum and plasma by liquid chromatography/mass spectrometry.

The European Union has regulated the use of non-steroidal anti-inflammatory drugs (NSAIDs) in animal production and requires its member states to detect their residues in different matrices. In this work, a detailed MS and MS/MS study by ion-trap mass spectrometry of fourteen NSAIDs is described. Two multi-residue reversed-phase LC/ESI-MS/MS methods were developed, one for the determination of salicylic acid, naproxen, carprofen, flurbiprofen, ibuprofen, niflumic acid and meclofenamic acid in the negative ion mode, and the other for the determination of ketoprofen, suxibutazone, diclofenac, mefenamic acid, tolfenamic acid, phenylbutazone and its metabolite oxyphenbutazone in the positive ion mode.