title: Development and validation of a method for the simultaneous extraction and separate measurement of oxytetracycline, florfenicol, oxolinic acid and flumequine from marine sediments.
abstract: A simple and rapid method for the detection and extraction of oxolinic acid, flumequine, florfenicol and oxytetracycline from marine sediments was developed and validated. The analytes were extracted from the marine sediment using a solution of oxalic acid diluted in methanol with sonication before detection by HPLC using a diode-array detector (florfenicol and oxytetracycline) and fluorescence (oxolinic acid and flumequine). The quantification limits (QL) were 100 ng/g for oxytetracycline and florfenicol and 5 ng/g for oxolinic acid and flumequine. The coefficients of variation of the repeatability and intermediate precision were less than 10% in all of the analytes. The calibration curves were linear between 50 and 500 ng/ml for oxytetracycline and florfenicol and 1 and 20 ng/ml for oxolinic acid and flumequine. The recuperation rate for the analytes was above 86%.
authors.affiliation: Instituto de Fomento Pesquero, División de Investigación en Acuicultura, Departamento de Salud Hidrobiológica, Balmaceda 252, Puerto Montt, Chile. luis.norambuena@ifop.cl
authors.forename: Luis
authors.initials: L
authors.lastname: Norambuena
authors.forename: Nuri
authors.initials: N
authors.lastname: Gras
authors.forename: Sergio
authors.initials: S
authors.lastname: Contreras
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D004784:Environmental Monitoring; D024841:Fluoroquinolones / Q000032:analysis*; D019015:Geologic Sediments / Q000737:chemistry*; D010093:Oxolinic Acid / Q000032:analysis*; D010118:Oxytetracycline / Q000032:analysis*; D013839:Thiamphenicol / Q000031:analogs & derivatives* / Q000032:analysis; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D024841:Fluoroquinolones; D014874:Water Pollutants, Chemical; C035534:florfenicol; D013839:Thiamphenicol; D010093:Oxolinic Acid; C012976:flumequine; D010118:Oxytetracycline
keywords: Florfenicol; Flumequine; HPLC; Marine sediment; Oxolinic acid; Oxytetracycline