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PubMed1987

Simultaneous determination of nalidixic acid, oxolinic acid and piromidic acid in fish by high-performance liquid chromatography with fluorescence and UV detection.

A simple and rapid method for the simultaneous determination of nalidixic acid (NA), oxolinic acid (OXA) and piromidic acid (PMA) in cultured fish has been developed by high-performance liquid chromatography (HPLC). The drugs were extracted with 0.1% metaphosphoric acid-methanol (6:4), followed by a Sep-Pak C18 clean-up procedure. The HPLC separation was carried out on a Kaseisorb LC ODS 300-5 column (25 cm x 4.6 mm I.D.) using 5 mM phosphate buffer-acetonitrile (6:4) as a mobile phase. A fluorescence detector was used for NA and OXA at the excitation wavelength of 325 nm and the emission wavelength of 365 nm and an ultraviolet detector at 280 nm for PMA. The calibration graphs were rectilinear from 1 to 10 ng for OXA, from 2 to 20 ng for NA and PMA. The recoveries of NA, OXA and PMA added to fish were 81.5-85.3, 83.7-88.7 and 80.9-84.9%, respectively, with high accuracy. The limits of detection were 0.01 micrograms/g for each drug.

Animals↗

PubMedDate not supplied

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 microns, 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%); and NAL, 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%).

Animals↗

PubMed1977