Rapid method for the determination of non-steroidal anti-inflammatory drugs in animal tissue by liquid chromatography-mass spectrometry with ion-trap detector.
A rapid and new liquid chromatography-mass spectrometry with ion-trap detection method for the determination of meloxicam (MLX), flunixin meglumine (FLU), carprofen (CPF), and tolfenamic acid (TOLF) in animal tissue is described. MRLs between 10 and 500 microg kg(-1) in muscle and between 65 and 1000 microg kg(-1) in liver, from different animal species have been established in the EU for these compounds. After chemical hydrolysis, an organic extraction from homogenised tissue was performed. Final extract was injected in a liquid chromatograph with an ion-trap mass spectrometer with electrospray interface. Four identification points (one precursor and two product ions) and a minimum of one ion ratio was monitored for each compound. For quantitative purposes flunixin-D3 (FLU-D3) was used as internal standard. The method was validated using fortified blank muscle and liver from different animal species according to the 2002/657/EC European decision criteria. The decision limits (CCalpha) and detection capabilities (CCbeta) were determined and their values were at concentrations near the MRL for each substance.
Igualada
Carmen
C
Laboratorio de Salud Pública de Valencia, Conselleria de Sanidad, Camí de la marjal s/n, 46470 Albal, Valencia, Spain. igualada_car@gva.es
Moragues
Francisco
F
Pitarch
Jorge
J
D000818:Animals; D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis*; D002227:Carbazoles / Q000032:analysis; D002417:Cattle; D002623:Chemistry Techniques, Analytical / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods*; D003002:Clonixin / Q000031:analogs & derivatives / Q000032:analysis; D006736:Horses; D007477:Ions; D008099:Liver / Q000187:drug effects / Q000378:metabolism; D013058:Mass Spectrometry / Q000379:methods*; D000077239:Meloxicam; D009132:Muscles / Q000187:drug effects / Q000378:metabolism; D013552:Swine; D013843:Thiazines / Q000032:analysis; D013844:Thiazoles / Q000032:analysis; D062367:ortho-Aminobenzoates / Q000032:analysis
D000894:Anti-Inflammatory Agents, Non-Steroidal; D002227:Carbazoles; D007477:Ions; D013843:Thiazines; D013844:Thiazoles; D062367:ortho-Aminobenzoates; C009500:tolfenamic acid; C014558:flunixin meglumine; C007005:carprofen; D003002:Clonixin; D000077239:Meloxicam