engleski

Determination of salicylic acid in milk using ultra performance liquid chromatography-tandem mass spectrometry

Non-steroidal anti-inflammatory drugs (NSAIDs) are widely used pharmaceuticals with analgesic, anti-inflammatory and antipyretic action. They are used for reducing pain, fever and treating rheumatic diseases. Recently, some NSAIDs are used for the prevention of cardiovascular diseases, stroke and also for the treatment of tumors. NSAIDs are used in veterinary practice as therapeutics e.g. mastitis treatment in dairy cows. Salicylic acid (SA) is one of the NSAIDs which belong to the salicylate group. These are natural products of plant metabolism. In this study milk samples were extracted with acetonitrile and clean up on SPE using an Evolute ABN. Determination of NSAIDs in milk is performed by the UPLC-MS/MS. Zorbax Eclipse XDB C18 (4.6 x 75 mm, 3.5 μm) column was used for separation of analytes. The method has been validated according to the Commission Decision 2002/657/EC. The following validation parameters for SA were defined: specificity, linearity, recovery 107, 0 %, limit of quantification (LOQ) 9, 27 μg kg-1, decision limit (CCα) 26, 1 μg kg-1 and detection capability (CCβ) 30, 3 μg kg-1. A total of 90 milk samples were analyzed for residues of NSAIDs. It has been found that 17 samples have values of SA above CCα and 11 samples between LOQ and CCα.

salicylic acid ; milk ; validation ; UPLC-MS/MS

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