engleski

Optimization Study of SPE-HPLC Pharmaceuticals Determination from Water Samples

Among the various emerging pollutants, pharmaceuticals are compounds of particular concern because of their physicochemical properties and appearance in the aquatic environment. The application of advanced measurement technologies to environmental analysis has allowed the determination of a broader range of compounds, including pharmaceuticals, and has therefore permitted more comprehensive assessment of environmental contaminants. The aim of this study was to develop an SPE sample preparation procedure and select the best HPLC column material for determination of pharmaceuticals from water samples. Investigated pharmaceuticals are ciprofloxacin, febantel, dexamethasone, sulfamethoxazole and trimethoprim. Different analytical columns were tested for the separation of the selected pharmaceuticals including different manufacturers (Agilent, Merck, Phenomenex, Shimadzu, Varian, Waters), with different size of columns (100-150 mm), inner diameter (2.1-4.6 mm) and particle size of sorbent (3.5-5 µm). They were tested with different mobile phases (acetic and formic acid, methanol, acetonitrile). A number of experiments were performed to optimize the mobile phase. Only on few columns the analytes were completely separated (co-elution, long retention times or peak broadening problems were observed). The pharmaceuticals were extracted applying different type of sorbents (C8, C18, Oasis HLB, Strata-X, SDB, etc.) from different manufacturers (Waters, Agilent, Phenomenex) and mass of sorbent (60mg, 200 mg, 500 mg) using different organic solvents (ethanol, acetonitrile, methanol) and different pH values of water samples (pH 2-9). The extraction efficiency was determined by high-performance liquid chromatography with selected HPLC column. Developed analytical method was validated for linearity, precision, repeatability, limit of detection (LOD), limit of quantification (LOQ) and recovery to confirm method suitability for determination of selected pharmaceuticals in wastewaters.

pharmaceuticals; wastewater; solid-phase extraction; high-performance liquid chromatography

nije evidentirano