Determination of Fluoroquinolone Antibacterial Agents in Sewage Sludge and Sludge-Treated Soil Using Accelerated Solvent Extraction Followed by Solid-Phase Extraction

Abstract

A method for the quantitative determination of human-use fluoroquinolone antibacterial agents (FQs) ciprofloxacin and norfloxacin in sewage sludge and sludge-treated soil samples was developed. The accelerated solvent extraction was optimized with regard to solvents and operational parameters, such as temperature, pressure, and extraction time. A 50 mM aqueous phosphoric acid/acetonitrile mixture (1:1) was found to be optimum in combination with an extraction temperature of 100 °C at 100 bar, during 60 and 90 min for sewage sludge and sludge-treated soil samples, respectively. A cleanup step using solid-phase extraction substantially improved the selectivity of the method. Overall recovery rates for FQs ranged from 82 to 94% for sewage sludge and from 75 to 92% for sludge-treated soil, with relative standard deviations between 8 and 11%. Limits of quantification were 0.45 and 0.18 mg/kg of dry matter for sewage sludge and sludge-treated soils, respectively. The presented method was successfully applied to untreated and anaerobically digested sewage sludges and sludge-treated soils. Ciprofloxacin and norfloxacin were determined in sewage sludges from several wastewater treatment plants with concentrations ranging from 1.40 to 2.42 mg/kg of dry matter. Therefore, contrary to what may be expected for human-use pharmaceuticals, FQs may reach the terrestrial environment as indicated by the occurrence of FQs in topsoil samples from experimental fields, to which sewage sludge had been applied.