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Application of SPE‐HPLC‐DAD and SPE‐TLC‐DAD to the determination of pesticides in real water samples
Author(s) -
Tuzimski Tomasz
Publication year - 2008
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200800368
Subject(s) - chromatography , high performance liquid chromatography , chemistry , repeatability , elution , analyte , calibration curve , solid phase extraction , chromatography detector , detection limit
Planar chromatography with diode array scanning (TLC‐DAD) and high‐performance chromatography with diode array detection (HPLC‐DAD) were used to screen water samples for pesticides. Pesticides were enriched from lake water samples by SPE on C18/SDB‐1, C18, C18 Polar Plus and cyanopropyl (CN) cartridges. The recovery rates were high for all extraction materials except for all pesticides on CN cartridges, for which the values were lower. SPE was used not only for preconcentration of analytes but also for their fractionation. The analytes were eluted first with methanol and then with dichloromethane. Methanol eluates were analysed by HPLC‐DAD, the dichloromethane eluates with TLC‐DAD. The method was validated for precision, repeatability and accuracy. The calibration plots were linear between 0.1 and 50.0 μg/mL for all pesticides, the correlation coefficients, r , were between 0.9992 and 1.000 as determined by HPLC‐DAD. In the TLC experiments, the best fit for the calibration lines was found when the calibration data were analysed using a second‐degree polynomial regression. Calibration plots lay between 0.1 and 17 μg/spot for all pesticides, the correlation coefficients, r , were between 0.9974 and 0.9997 determined by TLC‐DAD. The LOD was between 0.04 and 0.65 μg/spot (TLC‐DAD) and between 0.02 and 3.68 μg/mL (HPLC‐DAD).