Effective cleanup for the determination of six quinolone residues in shrimp before HPLC with diode array detection in compliance with the European Union Decision 2002/657/EC

Abstract

A high-performance liquid chromatographic method was developed for the determination of six quinolone residues (ciprofloxacin, enrofloxacin, sarafloxacin, oxolinic acid, nalidixic acid, and flumequine) in shrimp tissue samples. Separation was carried out by a LiChrospher® 100 RP-8e column, running at a 22 min gradient elution program, and the mobile phase consisted of citric acid (0.4 mol/L), acetonitrile and methanol. Detection was achieved by a diode array detector, monitoring at 255 and 275 nm. Sample preparation included initial extraction with citric acid solution and further clean-up by solid-phase extraction, employing Lichrolut RP-18 cartridges. Validation was performed according to the European Union Decision 2002/657/EC. The detection capability was 127.2 μg/kg for ciprofloxacin, 115.2 μg/kg for enrofloxacin, 126.2 μg/kg for sarafloxacin, 113.1 μg/kg for oxolinic acid, 125.2 μg/kg for nalidixic acid, and 239.0 μg/kg for flumequine. Recoveries ranged between 83.0 and 121.6%. The Youden test was applied to study the method ruggedness.

Voltammetric Analysis of Cephalexin and Cefazoline in Pharmaceutical Formulation and Biological Samples

“…Chromatographic methods using various detectors, due to simultaneous detection, accurate quantification, automation and the high selectivity based on the chemical structures of the analyte, have been the most commonly used for the detection of antibiotics (6)(7)(8). Furthermore, various techniques have been reported to determine these compounds including use of electrophoresis (9)(10)(11), diode array (12,13) or enzyme linked immunosorbent assay (ELISA) (14,15). However, there are some well-known disadvantages of these methods such as costly equipment and consumables, long analysis time, laborious sample preparation and the need for a well-trained technical personnel (16).…”

Detection of Antibiotics and Evaluation of Antibacterial Activity with Screen-Printed Electrodes

“…The most used methods for the detection of antibiotics are chromatographic [ 6 , 7 , 8 , 9 ], due to the automation, accurate quantification, simultaneous detection, and the high specificity based on the structural information of the analytes. Other methods for antibiotic determination include electrophoresis [ 10 , 11 , 12 , 13 , 14 ], diode array [ 15 , 16 ] or enzyme immunosorbent assay (ELISA) [ 17 , 18 , 19 ]. Meanwhile, for the detection of bacteria, the culture-based method remains the golden standard, although a good number of methods based on nucleic acid (e.g., based on polymerase chain reaction (PCR)) or immunologic reactions have been developed.…”