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

• Published in: Journal of Chromatography A Vol. 1172; no. 2; pp. 186 - 193
• Main Authors: Raich-Montiu, J., Folch, J., Compañó, R., Granados, M., Prat, M.D.
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 23.11.2007; Elsevier
• Subjects: Acetonitriles - chemistry; Analysis methods; Analytical chemistry; Antibacterial agents; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - instrumentation; Chromatography, High Pressure Liquid - methods; drug residues; Environment; Exact sciences and technology; extraction; Fluorescamine - chemistry; fluorescence; fluorimetry; high performance liquid chromatography; LC-fluorescence; microwave treatment; Natural water pollution; Other chromatographic methods; Pollution; Reproducibility of Results; Sensitivity and Specificity; Soil - analysis; Soil and sediments pollution; Soil Pollutants - analysis; soil pollution; Solid Phase Extraction; Spectrometry, Fluorescence - instrumentation; Spectrometry, Fluorescence - methods; Spectrometry, Mass, Electrospray Ionization - methods; Sulfonamides; Sulfonamides - analysis; Sulfonamides - isolation & purification; Veterinary Drugs - analysis; Veterinary Drugs - isolation & purification; Water - analysis; Water Pollutants, Chemical - analysis; water pollution; Water treatment and pollution; Environment; Sulfonamides; Water analysis; Soil analysis; Antibacterial agents; LC-fluorescence; Sulfadiazine; Chemical analysis; HPLC chromatography; Derivatization; Solvent extraction; Soil pollution; Sample preparation; Sulfadimethoxine; Antiinfectious; Quantitative analysis; Trace analysis; Fluorescence detector; Sulfonamide; Sulfadimidine; Soils; Reversed phase chromatography; Fluorescent labelling; Surface water; Water quality; Sulfachlorpyridazine; Water pollution; Antibacterial agent; Sulfametoxydiazine; Sulfaquinoxaline
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2007.10.010

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 6 ng g −1.