Confirmatory analysis of firocoxib in bovine milk by rapid resolution liquid chromatography tandem mass spectrometry

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2009-02, Vol.877 (5), p.541-546
• Main Authors: Dowling, Geraldine, Gallo, Pasquale, Regan, Liam
• Format: Article
• Language: English
• Subjects: 4-Butyrolactone - analogs & derivatives; 4-Butyrolactone - analysis; 4-Butyrolactone - chemistry; Analysis; Analytical, structural and metabolic biochemistry; Animals; Biological and medical sciences; Bovine milk; Cattle; Chromatography, Liquid; Decision limit; Detection capability; Firocoxib; Fundamental and applied biological sciences. Psychology; General pharmacology; Mass spectrometry; Medical sciences; Method validation; Milk - chemistry; Pharmacology. Drug treatments; Reproducibility of Results; Sulfones - analysis; Sulfones - chemistry; Tandem Mass Spectrometry - methods
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2008.12.059

A rapid method has been developed to analyse for firocoxib (FIRO) residue in bovine milk. Milk samples were extracted with acetonitrile and sample extracts were purified on Evolute™ ABN solid phase extraction cartridges. Aliquots were analysed by rapid resolution liquid chromatography tandem mass spectrometry (RRLC–MS/MS). The method was validated in bovine milk, according to the criteria defined in Commission Decision 2002/657/EC. The decision limit (CCα) was 1.18 ng/mL and for the detection capability a (CCβ) value of 2.02 ng/mL was obtained. The measurement uncertainty of the method was 27%. Fortifying bovine milk samples ( n = 18) in three separate assays, show the accuracy of the method to be between 96 and 105%. The precision of the method, expressed as RSD values for the within-lab reproducibility at the three levels of fortification (5, 7.5 and 10 ng/mL) was less than 11% respectively.