## Abstract Metabolite identification is a key step for metabonomics study. A fully automated hyphenation of HPLC‐diode‐array detector (DAD) mass spectrometry (MS) solid phase extraction (SPE)–NMR spectroscopy (HPLC‐DAD‐MS‐SPE‐NMR) is one of the most efficient methods to determine the structure of
Application of SPE-HPLC-DAD and SPE-TLC-DAD to the determination of pesticides in real water samples
✍ Scribed by Tomasz Tuzimski
- Book ID
- 102924698
- Publisher
- John Wiley and Sons
- Year
- 2008
- Tongue
- English
- Weight
- 756 KB
- Volume
- 31
- Category
- Article
- ISSN
- 1615-9306
No coin nor oath required. For personal study only.
✦ Synopsis
Abstract
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).
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