title: Development and validation of two multiresidue liquid chromatography tandem mass spectrometry methods based on a versatile extraction procedure for isolating non-steroidal anti-inflammatory drugs from bovine milk and muscle tissue.
abstract: The main difficulties in analysing non-steroidal anti-inflammatory drugs (NSAIDs) in food and biological samples are due to the tight non-covalent interactions established with matrix proteins and the amount of occurring fatty material. The present paper describes an effective extraction procedure able to isolate fifteen NSAIDs (acetaminophen, salicylic acid, ibuprofen, diclofenac, flunixin and its metabolite 5-hydroxy-flunixin, nimesulide, phenylbutazone, meclofenamic acid, tolfenamic acid, meloxicam, carprofen, ketoprofen, naproxen and etodolac) from bovine milk and muscle tissue through two succeeding steps: (a) deproteinisation/extraction with organic solvent, essential to lower the medium dielectric constant and, therefore, to release the analytes from matrix; (b) SPE clean-up on OASIS cartridges. Lipids were easily removed during low-temperature centrifugations. The advantages of the developed procedure pertain to the efficient removal of the fat substances (very low matrix effect and high recovery yields) and its versatility, since it can be applied both to milk and muscle with few adjustments due to the diversity of the two matrices. Ion-pairing reversed-phase chromatography combined with the negative electrospray detection was able to achieve low detection capabilities (CCβs) for all analytes and, in particular, for diclofenac whose Maximum Residue Limit (MRL) in milk is 0.1 μg kg(-1). The methods were validated according to the guidelines of the Commission Decision 2002/657/EC and then applied for a small monitoring study. A number of samples showed traces of salicylic acid (SA), but its occurrence was not ascribed to a misuse of drugs (aspirin, salicylic acid) since SA, accumulating in plants in response to a pathogen attack, may be introduced into the food chain.
authors: Department of Chemistry, Faculty of Mathematical, Physical and Natural Sciences, Sapienza University of Rome, Rome, Italy.
authors: Alessandra
authors: A
authors: Gentili
authors: Fulvia
authors: F
authors: Caretti
authors: Simona
authors: S
authors: Bellante
authors: Lucia
authors: L
authors: Mainero Rocca
authors: Roberta
authors: R
authors: Curini
authors: Alessandro
authors: A
authors: Venditti
mesh_terms: D000818:Animals; D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis / Q000302:isolation & purification*; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods; D008055:Lipids / Q000302:isolation & purification; D008892:Milk / Q000737:chemistry*; D009132:Muscles / Q000737:chemistry*; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal; D008055:Lipids