The development of a microwave-assisted extraction method for the determination of sulfonamide antibiotics in sediments and soils

Abstract

A microwave-assisted extraction technique was developed for the determination of nine sulfonamide antibiotics (sulfaguanidine, sulfacetamide, sulfadiazine, sulfathiazole, sulfapyridine, sulfamethazine, sulfamerazine, sulfamethoxazole, and sulfadimethoxine) in six sediments and soils of varying organic carbon content. Method optimization was performed using Lake Erie sediment and revealed the optimum extraction solvent to be methanol, with an extraction time of 45 min. After extraction, samples were “cleaned up” via filtration and quantified using LC-MS/MS spectroscopy. Method calibration curves were constructed in each environmental solid with sulfonamides ranging from 10 to 2000 ng/g; method detection limits were typically in the sub- to low nanograms per gram range. Method validation entailed spiking each solid at three different concentrations spanning the calibration curve (40, 300, and 800 ng/g); generally, method accuracy for spiked solids exceeded 80%, with precision being within 20%. Finally, we extracted sulfonamides from environmental solids (two sediments and one soil) that had been aged for 21 days and found that our method accuracy remained in excess of 80%. Moreover, absolute recoveries generally agreed with method accuracies (at the 95% confidence interval) in all environmental solids, demonstrating the efficiency of our microwave-assisted extraction procedure and its suitability for application to environmental samples.