Simultaneous Determinaton of Fluoroquinolones in Feed by Liquid Chromatography with Fluorescence Detection

Abstract

An HPLC method with fluorescence detection (HPLC-FLD) was developed for the simultaneous quantitative determination of enrofloxacin, ciprofloksacin, sarafloxacin, and difloxacin in feed. The samples were extracted with 0.25% formic acid in ultrasonic bath and purified by solid phase extraction (SPE) on Strata-X cartridges. The samples were analysed on Luna C8 liquid chromatography column with gradient programme by acetonitrile and 0.025 M phosphoric acid with 0.0025 M sodium 1- heptanesulfonate monohydrate. The method was successfully validated according to the requirements of the European Decision 2002/657/EC. Recoveries of the components from spiked feed samples ranged from 55%-70%. Repeatability was <7%. The method presented here proved to be efficient, rapid, and a selective approach for determination of fluoroquinolones in feed.

Determinaton of enrofloxacin and ciprofloxacin in albumin and freeze-dried-eggs by liquid chromatography with fluorescence detection

“…However, data from the literature and Rapid Alert System for Food and Feed (RASFF) indicated that there were incidents of ENR illegal use in laying hens' therapy (15). Many analytical methods for determination of ENR in animal tissues, feed, milk, and egg have been described (6,10,13,14). Nevertheless, none of the developed methods concerns analysis of these compounds in albumin and freeze-dried-eggs.…”

A modified QuEChERS method development to analyze tylosin and metronidazole antibiotics residue in shrimp (Penaeus monodon) using LC-ESI MS/MS

“…The results of our experiments showed that 0.1% formic acid was the best additive for increasing peak resolution and sensitivity. Most published methods used acetonitrile as an organic solvent mobile phase for the analysis of an antibacterial compound (Gbylik et al, 2012). In this study, the best results were obtained utilizing a gradient elution and a chromatographic column with acetonitrile and 0.1% formic acid in Milli-Q water.…”

Systematic optimization of an SPE with HPLC-FLD method for fluoroquinolone detection in wastewater

“…In previously reported methods, the excitation/emission wavelengths for most FQs were generally set to 278/445 nm or 280/465 nm [5,32]; in addition, a few methods have used excitation/emission wavelengths of 293/500 nm for LEV and MOX [37]. A single set of excitation and emission wavelengths does not allow optimized detection of all FQs.…”

“…Mobile phases containing nonvolatile acids or salts have been shown to suppress FQ ionization [7,17,27,28]. As many chromatography methods [5,7,15,[29][30][31][32][33][34] have employed phosphate buffers to reduce FQ peak asymmetry, this eluent limitation can negatively affect FQ peak shape during LC-MS/MS analysis.…”

“…Previous reports have focused on developing HPLC-UV and -FLD methods for analysis of FQ antibiotics in various matrices, including blood, urine, water, wastewater, soil, and animal feed [5,17,18,22,[30][31][32][35][36][37][38][39][40][41][42]. While UV detectors are limited by relatively high limits of detection, HPLC-FLD has been shown to be quite sensitive for determination of FQ antibiotics; however, these methods have not been fully optimized in terms of analyte resolution and low limits of detection/quantitation.…”