Analytical methods for the determination of some selected 4-quinolone antibacterials

A comprehensive review with 337 references for the analysis of some selected 4-quinolone drugs belonging to the first and second generations since 2006 up till now is presented. This group includes nalidixic acid, oxolinic acid, piromidic acid, pipemidic acid and rosoxacin from the first generation and enoxacin, fleroxacin, nadifloxacin, pefloxacin and rufloxacin from the second generation. The review covers most of the methods described for the analysis of these drugs, either

Liquid Chromatographic Determination of Flumequine, Nalidixic Acid, Oxolinic Acid, and Piromidic Acid Residues in Catfish (Ictalurus punctatus)

A peer-verified, liquid chromatographic (LC) method for simultaneous determination of residues of flumequine (FLU), nalidixic acid (NAL), oxolinic acid (OXO), and piromidic acid (PIR) in catfish muscle is presented. Sample workup involves homogenizing tissue with acetone, defatting with hexane, and extracting quinolones into chloroform. Sample is purified further by partitioning into base and then subsequently back-extracting into chloroform after acidifying the aqueous phase. After solvent is evaporated, the residue is diluted with mobile phase, and analytes are introduced into an LC system where separations are made with a 5 |am, reversed- phase polymer column and an isocratic, buffered acetonitrile- tetrahydrofuran mobile phase. Determinations are made by UV detection at 280 nm for PIR and by fluorescence detection (excitation at 325 excitation and emission at 365 nm) for the other 3 analytes. Each quinolone was used to fortify catfish muscle at 5, 10, 20, 40, and 80 ng/g. The following recoveries and relative standard deviation (RSD) values represent an average of the 5 levels for each analyte: FLU, 79.7℅ (RSD = 5.7℅); OXO, 80.8℅ (RSD = 6.3℅); PIR, 75.0℅ (RSD = 5.9℅); andNAL, 87.1℅ (RSD = 10%). Assay of 5 levels (base incurred catfish, plus 4 dilutions with control catfish) of catfish muscle incurred with the 4 quinolones gave the following averages: FLU: base, 198 ng/g (RSD = 2.3℅); dilutions, 98.0 ng/g (RSD = 4.2℅), 61.6 ng/g (RSD = 4.4℅), 21.6 ng/g (RSD = 2.8℅), 9.24 ng/g (RSD = 8.7℅); OXO, base, 257 ng/g (RSD = 6.9℅); dilutions, 146 ng/g (RSD = 5.5℅), 95.0 ng/g (RSD = 4.1℅), 30.7 ng/g (RSD = 3.8%), 13.7 ng/g (RSD = 4.6%); PIR, base, 22.1 ng/g (RSD = 4.2%); dilutions, 13.7 ng/g (RSD = 6.7℅), 6.49 ng/g (RSD = 15℅), 2.65 ng/g (RSD =15℅); and NAL, base, 75.1 ng/g (RSD = 3.8℅); dilutions, 42.3 ng/g (RSD = 5.1℅), 24.1 ng/g (RSD = 6.3℅), 8.59 ng/g (RSD = 4.8℅). A second multiresidue analysis of the 4 quinolones was performed by an outside analyst. Average recoveries from catfish fortified at 5, 10, 20, and 40 ng/g were FLU, 75.9℅ (RSD = 4.0℅); OXO, 84.0℅ (RSD = 5.5℅); NAL, 85.6℅ (RSD = 8.9℅); and PIR, 66.2℅ (RSD = 8.7℅).