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

被引：14
|
作者：
Dowling, Geraldine [1 ]
Gallo, Pasquale [2 ]
Regan, Liam [1 ]
机构：
[1] Stat Lab, Celbridge, Kildare, Ireland
[2] Ist Zooprofilat Sperimentale Mezzogiorno, I-80055 Naples, Italy
来源：
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2009年 / 877卷 / 5-6期
关键词：
Firocoxib; Bovine milk; Method validation; Decision limit; Detection capability; Mass spectrometry; NONSTEROIDAL ANTIINFLAMMATORY DRUGS; IN-VIVO EFFICACY; CYCLOOXYGENASE-2; INHIBITOR; HORSE;
D O I：
10.1016/j.jchromb.2008.12.059
中图分类号：
Q5 [生物化学];
学科分类号：
071010 ; 081704 ;
摘要：
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 (TM) 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 (CC alpha) was 1.18 ng/mL and for the detection capability a (CC beta) 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. (C) 2009 Elsevier B.V. All rights reserved.
引用
收藏
页码：541 / 546
页数：6
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