Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume 44,
Number 10, November/December 2006, pp.585-590
Multi-Residue Determination of Non-Steroidal Anti-Inflammatory
Drug Residues in Animal Serum and Plasma by HPLC and Photo-Diode
Array Detection
Pasquale Gallo[1], Serena Fabbrocino[1], Floriana
Vinci[1], Maurizio Fiori[2], Vincenzo Danese[1], Antonella Nasi[1],
and Luigi Serpe[1]
[1]Istituto Zooprofilattico Sperimentale del Mezzogiorno, Via
Salute 2–80055 Portici, NA, Italy and
[2]Istituto Superiore di Sanità, viale Regina Elena 299–00161,
Roma, Italy
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. These compounds are chosen
as the most representative of the different NSAID chemical sub-classes.
The DAD analysis allows the confirmation of all drugs on the basis
of their own UV–vis spectrum, according to the requirements
of the European Council Decision 2002/657/EC. Moreover, the method
is in-house validated, evaluating mean recoveries, specificity,
repeatability, and within-laboratory reproducibility as the performance
parameters required by the Decision. The results of this study
indicate the method is specific and repeatable, with the mean
percentage recoveries of the drugs ranging between 72.5% and 104.5%.
Only salicylic acid has poor recovery, with results ranging between
36.3% and 54.9%.
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