Anal. Chem. 1996, 68, 1905-1909
Liquid Chromatography Combined with Tandem Mass Spectrometry for the Confirmation of Sarafloxacin in Catfish Tissue James B. Schilling,* Steven P. Cepa, Stanley D. Menacherry, Lalit T. Bavda, Beatrice M. Heard, and Brenda L. Stockwell
Abbott Laboratories, 1400 North Sheridan Road, North Chicago, Illinois 60064
A specific chromatographic LC/MS/MS assay is described for the confirmatory identification of residues of sarafloxacin, an arylfluoroquinolone antibacterial agent, in catfish tissue. This confirmatory method takes advantage of the specificity provided by sample preparation, liquid chromatography, and tandem mass spectrometry. This kind of multidimensional analysis is commonly used in environmental, pharmacokinetic, residue, and other studies. However, we demonstrate the addition of a previously unreported criterion, the use of ion ratio ranges from the tandem mass spectrometry (MS/MS) experiment as an aid in confirmation. Using the described method, we were able to achieve MS/MS product ion ratios with 1900, which corresponds to S/N > 30. The parent and three diagnostic ions’ normalized areas were all within (7% of a the standards product ions, normalized areas. In addition, statistical evaluation of the data (n ) 23) was performed, resulting in means (standard deviations) of 54.44% (2.7) for the 386 m/z, 16.50% (1.0) for the 342 m/z, and 26.65% (1.7) for the 299 m/z. These results demonstrate that it is possible to use a criterion of
