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Online trace enrichment to determine pyrethroids in river water by HPLC with column switching and photochemical induced fluorescence detection
Authors:Martínez Galera Maria  Barranco Martínez Dolores  Parrilla Vázquez Piedad  Gil García Maria Dolores
Affiliation:Department of Hydrogeology and Analytical Chemistry, University of Almería, La Ca?ada de San Urbano, Spain. mmartine@ual.es
Abstract:The potential of online trace enrichment on a highly apolar short column in LC was evaluated for the determination of pyrethroids in river water. Twelve millilitres of water samples, modified with 8 mL ACN (ACN/water 40:60, v/v), were passed through 50 x 4.6 mm ID first separation column packed with 5 microm Hypersil Elite C18. Pesticides were preconcentrated in this column while the matrix background was eluted to waste. Separation of pesticides was performed on a 3.5 microm symmetric C18 column (250 x 4.6 mm ID) with an ACN step gradient as mobile phase and fluorescence detection was used after postcolumn derivatization by using UV light. The use of photochemically induced fluorescence for detection improved sensitivity and selectivity. Quantification limits ranged from 0.05 to 0.1 microg/L and pesticide recoveries at two concentration levels (0.1 and 0.5 microg/L) were between 93.1 and 118.6%, with RSD between 2.5 and 7.5% (n = 3) in river water samples. No matrix effect was detected.
Keywords:Liquid chromatography  Online SPE enrichment  Pyrethroids  River waters
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