engleski

Development and validation of sample preparation procedures for quantification of veterinary pharmaceuticals in sediment

Sediments act as a potential receiver for many hazardous chemicals, including the pharmaceuticals, which have been emitted to surface waters. From these reasons it is necessary to monitor the pharmaceuticals in sediment with adequate analytical techniques like chromatographic methods. Chromatographic methods demand good and delicate sample preparation procedure because of complex sediment matrix [1-5]. Simple and sensitive methods for simultaneous analysis of eight veterinary pharmaceuticals: antihelmintics (albendazole, febantel and levamisole), local anesthetics (lidocaine and procaine), macrolide antibiotic tylosin, and glucocorticosteroids (dexamethasone and hydrocortisone) in sediment samples were developed and validated. The target compounds were extracted using microwave assisted extraction (MAE), ultrasound solvent extraction (USE), pressurized liquid extraction (PLE), matrix solid-phase dispersion (MSPD) on C18 sorbens and extraction by agitation (EA). The quantitative analysis was performed by liquid chromatography with diode array detector. The developed methods were validated through the estimation of the linearity, sensitivity, repeatability, reproducibility and matrix effects. The external standard method and standard addition method were used for quantification in order to efficiently correct matrix effects. Despite the strong matrix interferences, the recoveries were generally higher than 50% and the detection and quantification limits were very low. Beside the very good sensitivity provided by HPLC-DAD, an important characteristic of the all developed methods is that all the target compounds can be simultaneously extracted, treated and analyzed. Hence, it can be used for routine analysis of veterinary pharmaceuticals in sediment.

sediment; veterinary pharmaceuticals; sample preparation

This work has been supported by Croatian Ministry of Science, Education and Sports Project: 125-1253008-1350 Development of advanced analytical methods for pharmaceuticals determination in the environment and Bilateral project HR-SLO: Determination of toxicity and physico-chemical properties of pharmaceuticals.