Multi-residue determination of antibiotics in fish by liquid chromatography-tandem mass spectrometry

Abstract

A multi-residue method for the determination of 34 antibacterial drugs (three aminoglycosides, nine β-lactams, nine fluoroquinolones, three macrolides, five sulfonamides, trimethoprim and four tetracyclines) in fish samples by LC-MS/MS was developed. The procedure enables the isolation of residues based on double extraction of the fish sample with m-phosphoric acid and heptafluorobutyric acid as an ion-pair agent and acetonitrile. All compounds were determined at the same time on a C18 column with gradient elution. The method was validated according to the requirements of European Decision 2002/657/EC. Specificity, recovery, repeatability, within-laboratory reproducibility, decision limit CCα and detection capability CCβ were calculated. CCα ranged from 55.3 to 1085 µg kg(-1) and CCβ ranged from 59.5 to 1141 µg kg(-1). The overall recoveries were from 96% to 111% with respect to the internal standards.

Effect of doxycycline concentrations in chicken tissues as a consequence of permanent exposure to enrofloxacin traces in drinking water

“…The optimisations of instrumental parameters and sample preparation procedures were based on the available literature (8,10,14,15,29) and our experience with antibiotic residue analyses (4,16). The developed method provided quantitative doxycycline, enrofloxacin, and ciprofloxacin determination results.…”

Simultaneous determination of ten aminoglycoside antibiotics in aquatic feeds by high‐performance liquid chromatography quadrupole‐orbitrap mass spectrometry with pass‐through cleanup

“…The sheath gas and auxiliary gas flow rate was 40 and 5 psi, respectively. The mass spectra were acquired with full MS‐data dependent MS/MS (full MS‐ddMS) mode. The full scan mass spectra were recorded in the range of 100 to 700 m/z at a resolution of 70,000, with automatic gain control (AGC) target of 1.0 × 10, and maximum injection time (IT) of 100 milliseconds.…”

“…Aminoglycosides (AGs) are broad‐spectrum antibiotics, which are particularly active against both gram‐positive and gram‐negative bacteria . In aquaculture, AGs have been widely used as veterinary drugs to treat bacterial infectious diseases . In recent years, AGs have also been employed as a feed additive to promote growth and increase feed efficiency, because it can facilitate absorption of nutrition in animals .…”

High-throughput method for macrolides and lincosamides antibiotics residues analysis in milk and muscle using a simple liquid–liquid extraction technique and liquid chromatography–electrospray–tandem mass spectrometry analysis (LC–MS/MS)

“…The NRCP is an attribution of Ministry of Agriculture, Livestock and Food Supply (MAPA) [9,10]. Many studies have reported methodologies based on liquid chromatography couple to mass spectrometry in single or tandem mode (LC-MS and LC-MS/MS, respectively) to determine macrolides and lincosamides residues in milk [11][12][13][14] and muscle [15][16][17][18][19][20][21], and also in different matrices, such as honey [22,23], eggs [24], fish [25] and kidney [26,27]. These compounds are routinely included in multiresidue methodologies [14,16,19,[22][23][24][28][29][30][31], and there is minor publications of macrolides class only [32,33] or macrolides and lincosamides only [21].…”