Analysis of trace levels of sulfonamides in surface water and soil samples by liquid chromatography-fluorescence.
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).
Raich-Montiu
J
J
Departament de Química Analítica, Universitat de Barcelona, Martí i Franquès 1, 08028 Barcelona, Spain.
Folch
J
J
Compañó
R
R
Granados
M
M
Prat
M D
MD
D000097:Acetonitriles / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation* / Q000379:methods; D005450:Fluorescamine / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012987:Soil / Q000032:analysis*; D012989:Soil Pollutants / Q000032:analysis*; D052616:Solid Phase Extraction; D013050:Spectrometry, Fluorescence / Q000295:instrumentation* / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D013449:Sulfonamides / Q000032:analysis* / Q000302:isolation & purification; D019155:Veterinary Drugs / Q000032:analysis / Q000302:isolation & purification; D014867:Water / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis*
D000097:Acetonitriles; D012987:Soil; D012989:Soil Pollutants; D013449:Sulfonamides; D019155:Veterinary Drugs; D014874:Water Pollutants, Chemical; D014867:Water; D005450:Fluorescamine; C032159:acetonitrile