Multiresidue Method for the Determination of Quinolone Antibiotics in Bovine Raw Milk by Capillary Electrophoresis-Tandem Mass Spectrometry
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- 作者：Francisco J. Lara ; Ana M. Garcí ; a-Campañ ; a ; Fermí ; n Alé ; s-Barrero ; Juan M. Bosque-Sendra ; Luis E. Garcí ; a-Ayuso
- 刊名：Analytical Chemistry
- 出版年：2006
- 出版时间：November 15, 2006
- 年：2006
- 卷：78
- 期：22
- 页码：7665 - 7673
- 全文大小：279K
- 年卷期：v.78,no.22(November 15, 2006)
- ISSN：1520-6882
文摘
A new analytical method based on capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) isproposed and validated for the identification and simultaneous quantification of eight quinolones for veterinaryuse in bovine raw milk. The studied quinolones includedanofloxacin, sarafloxacin, ciprofloxacin, marbofloxacin,enrofloxacin, difloxacin, oxolinic acid, and flumequine,whose contents are regulated by the EU Council Regulation no. 2377/90 in animal edible tissues. Differentparameters (i.e., separation buffer composition and electrospray conditions) were optimized in order to obtainboth an adequate CE separation and a high sensitivity,using experimental design methodology to consider theinteractions among the studied variables. MS/MS experiments using an ion trap as analyzer operating in themultiple reaction monitoring mode were carried out toachieve the minimum number of identification pointsaccording to the 2002/657/EC European Decision. Forthe quantification in bovine raw milk samples, a two-stepsolid-phase extraction procedure was developed usingOasis MAX and HLB cartridges without protein precipitation. Satisfactory results were obtained in terms of linearity (r2 between 0.989 and 0.992) and precision (RSDbelow 18%). The limits of detection and quantification(below 6 and 24 ppb, respectively) were in all cases lowerthan the maximum residues limits tolerated for thesecompounds in milk, the recoveries ranging from 81 to110%, indicating the potential of the CZE-MS/MS for theanalysis of regulated quinolone antibiotics in the foodquality and safety control areas.