Analysis of trace levels of sulfonamides in surface water and soil samples by liquid chromatography-fluorescence

Abstract: Methods are reported for determining six sulfonamides used as veterinary drugs in water and soil samples. Analytes are isolated from water samples by solid-phase extraction on HBL cartridges and pre-concentration factors of up to 250 were obtained. Soil samples are treated using microwave-assisted extraction of analytes with acetonitrile and further clean up by solid-phase extraction. Determination is carried out by high-performance liquid chromatography using fluorimetric detection with precolumn derivatization with fluorescamine. The separation of the derivatized sulfonamides is performed on an octadecyl column using binary gradient elution with acetate buffer/acetonitrile mixtures. For water analysis, the detection limits of the whole process are in the low nanogram per liter level and recovery rates range from 70 to 104%, with standard deviations 2–11%. For soil analysis, extraction efficiency is evaluated using three soil samples with different physicochemical characteristics. Recovery rates range from 60 to 98% and detection limits are between 1 and 6ngg−1. [Copyright &y& Elsevier]