Liquid Chromatography Combined with Tandem Mass Spectrometry for the Confirmation of Sarafloxacin in Catfish Tissue

Abstract

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 <7% variation during 1 day of analysis for over 25 injections. We believe the addition of this criterion will increase the scientific certainty of the confirmatory method.

Electrospray ionization and collision-induced dissociation of antibiotic polyether ionophores

“…Commonly, guidelines for confirmatory analyses suggest at least three structure-diagnostic ions per compound, including the [MH] ion. 28,29 Confirmation criteria for MS/MS experiments are less clearly defined. As pointed out by Schilling and co-workers, 29 choice of diverse product ions is necessary for a high degree of specificity in the MS/MS analysis.…”

“…28,29 Confirmation criteria for MS/MS experiments are less clearly defined. As pointed out by Schilling and co-workers, 29 choice of diverse product ions is necessary for a high degree of specificity in the MS/MS analysis. In this study, three structure-specific CID transitions, based on the dissociation pathways described in the previous section, were chosen for detection in the multiplereaction monitoring mode.…”

A review of current applications of mass spectrometry for biomarker/molecular tracer elucidations

“…Various experimental systems have been described and used to evaluate, for example, coal-liquefaction products in terms of the number of condensed rings separated by the HPLC into fractions that were further separated and analyzed by LC/MS (Dark, McFadden, & Bradford, 1977;McFadden et al, 1977;McFadden, 1982). Currently, HPLC-MS is used to elucidate the structures of polar and highly functionalized biomarkers and natural products (McFadden et al, 1979;Voyksner, 1994;Thomson, 1998;Harada & Fujii, 2000) and organic compounds in environmental samples (Schilling et al, 1996;Suter, Riediker, & Giger, 1999).…”

Liquid chromatographic separation of fluoroquinolone antibacterials used as veterinary drugs

“…The selected additives include complexing acids, such as citric [19] and oxalic [20], anionic ion-pairing agents such as sodium perchlorate and sodium dodecylsulfate (SDS) [21], and quaternary ammonium salts such as tetrabutylammonium (TBA) bromide [22]. The pH was maintained at 3.5, and thus, when TBA, SDS and NaC104 were used as modifiers, a formic buffer solution was added to regulate pH.…”