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A method for the quantitative determination of humanuse 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 degrees 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.
Golet et al. (Tue,) studied this question.