Determination of pesticides in water samples from the Wieprz-krzna Canal in the Leczyńsko-Włodawskie Lake District of southeastern Poland by thin-layer chromatography with diode array scanning and high-performance column liquid chromatography with diode array detection.
High-performance thin-layer chromatography with diode array scanning (TLC-DAD) and high-performance column liquid chromatography with a diode array detector (HPLC-DAD) were used to screen water samples for pesticides. Atrazine, clofentezine, chlorfenvinphos, hexaflumuron, terbuthylazine, lenacyl, neburon, bitertanol, and metamitron were enriched from canal water samples by solid-phase extraction (SPE) on octadecyl silane (C18)/styrene-divinylbenzene-1, C18, C18 Polar Plus, and cyanopropyl (CN) cartridges. Recovery rates were high for all extraction materials except CN, for which values for all pesticides were lower. SPE was used for both preconcentration and fractionation of the analytes. Analytes were eluted by means of methanol and dichloromethane. Methanol eluates were analyzed by HPLC-DAD and dichloromethane eluates by TLC-DAD. The method was validated for precision, repeatability, and accuracy. Calibration graphs were linear between 0.1 and 50.0 microg/mL for all pesticides, and correlation coefficient (r) values were between 0.9994 and 1.000 as determined by HPLC-DAD. Calibration graphs were linear between 0.1 and 1.5 microg/spot for all pesticides, and r values were between 0.9899 and 0.9987 as determined by TLC-DAD. The limit of detection was between 0.04 and 0.23 microg/spot for TLC-DAD and 0.02 and 0.45 microg/mL for HPLC-DAD.
Tuzimski
Tomasz
T
Medical University, Department of Physical Chemistry, Faculty of Pharmacy, Lublin, Poland. tomasz.tuzimski@am.lublin.pl
D002138:Calibration; D002722:Chlorobenzenes / Q000032:analysis; D002851:Chromatography, High Pressure Liquid; D002855:Chromatography, Thin Layer; D003720:Densitometry; D006540:Herbicides / Q000032:analysis; D007202:Indicators and Reagents; D007306:Insecticides / Q000032:analysis; D010573:Pesticide Residues / Q000032:analysis*; D010575:Pesticides / Q000032:analysis*; D011044:Poland; D012015:Reference Standards; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet; D014874:Water Pollutants, Chemical / Q000032:analysis*; D014881:Water Supply / Q000032:analysis*
D002722:Chlorobenzenes; D006540:Herbicides; D007202:Indicators and Reagents; D007306:Insecticides; D010573:Pesticide Residues; D010575:Pesticides; D014874:Water Pollutants, Chemical; C062106:clofentezine