On-line flow-through extraction-preconcentration-large volume injection reversed-phase liquid chromatography method for trace determination of selected pyrethroids in Slovak soil micro-samples
2009
Chalányová, M., Comenius Univ., Bratislava (Slovak Republic) | Hutta, M., Comenius Univ., Bratislava (Slovak Republic) | Pagáč, M., Comenius Univ., Bratislava (Slovak Republic)
A rapid micro-analytical multiresidue method has been developed for the analysis of selected pyrethroids (cypermethrin and permethrin) in a micro-sample of soil (mass around 200 mg). The method is based on the on-line flow-through extraction of soil micro-samples (packed into a short glass column) with a methanol-aqueous citric acid buffer mixture, successive on-line solid-phase extraction preconcentration (SPE) of analytes from the extract and on-line RP-HPLC analysis with UV photometric detection. The separation of pyrethroids was performed on a Purospher RP-18e column with methanol-water binary mobile phase. Effects of sorbent placed at bottom of short column holding the soil sample and different kinds of on-line SPE columns were tested. Beside the influence of volume of the effluent on the pyrethroids recovery was also studied. Calibration curves were linear over the range assayed from 0.01 to 0.2 microg per mL with correlation coefficients of linear regression in the range 0.998-0.999. Recovery studies were carried out at 0.25-1.00 microg per g dry soil fortification level and obtained recoveries were for cypermethrin 56-59% and for permethrin 58-63%. Achieved detection limits of studied synthetic pyrethroids were 3.7 ng per g of cypermethrin and 3.6 ng per g of permethrin, respectively.
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