Development and validation of a method for the simultaneous extraction and separate measurement of oxytetracycline, florfenicol, oxolinic acid and flumequine from marine sediments

Norambuena, Luis; Gras, Nuri; Contreras, Sergio

Development and validation of a method for the simultaneous extraction and separate measurement of oxytetracycline, florfenicol, oxolinic acid and flumequine from marine sediments

2013

Norambuena, Luis | Gras, Nuri | Contreras, Sergio

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 100ng/g for oxytetracycline and florfenicol and 5ng/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 500ng/ml for oxytetracycline and florfenicol and 1 and 20ng/ml for oxolinic acid and flumequine. The recuperation rate for the analytes was above 86%.

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