Preconcentration of pharmaceuticals residues in sediment samples using microwave assisted micellar extraction coupled with solid phase extraction and their determination by HPLC-UV.
An analytical method combining microwave assisted micellar extraction (MAME) and solid phase extraction (SPE) has been developed to extract and preconcentrate a selected group of eight pharmaceutical compounds in sediment samples prior to their determination using liquid chromatography with an UV-DAD detector. A non-ionic surfactant, Polyoxyethylene 10 lauryl ether (POLE) was used for the MAME extraction and the different parameters for the optimization process were studied. Then, SPE was used to clean-up and preconcentrate the target analytes in the extract, prior to their determination using HPLC-UV. The method was applied to the determination of the selected pharmaceuticals compounds in several kinds of sediment samples with different characteristics. Relative recoveries for spiked sediment samples were over 70% and relative standard deviations (RSDs) were under 11% for all recoveries tested. Detection limits between 4 and 167ngg(-1) were obtained. The method was validated using Soxhlet extraction procedure.
Cueva-Mestanza
R
R
Department of Chemistry, University of Las Palmas de Gran Canaria, 35017 Las Palmas de Gran Canaria, Spain.
Sosa-Ferrera
Z
Z
Torres-Padrón
M E
ME
Santana-Rodríguez
J J
JJ
D002138:Calibration; D055598:Chemical Phenomena; D002627:Chemistry, Physical; D002851:Chromatography, High Pressure Liquid; D004350:Drug Residues / Q000032:analysis*; D019015:Geologic Sediments / Q000032:analysis*; D007202:Indicators and Reagents; D008823:Micelles; D008872:Microwaves; D000077423:Polidocanol; D011092:Polyethylene Glycols; D011786:Quality Control; D012987:Soil / Q000032:analysis; D012989:Soil Pollutants / Q000032:analysis*; D052616:Solid Phase Extraction; D013030:Spain; D013056:Spectrophotometry, Ultraviolet
D007202:Indicators and Reagents; D008823:Micelles; D012987:Soil; D012989:Soil Pollutants; D000077423:Polidocanol; D011092:Polyethylene Glycols