Determination of carbamates at trace levels in water and cucumber by capillary liquid chromatography
A sensitive and reliable method using capillary HPLC with UV-diode array detection (DAD) has been developed and validated for trace determination of carbamate pesticides in cucumber and environmental water samples. The analytes, including carbofuran, carbaryl, methiocarb, promecarb, benthiocarb and fenoxycarb, present legal residue levels regulated by the EU Council Directive 98/83/EC on drinking water and by the Regulation (EC) No. 396/2005 on vegetables. A previous off-line solid-phase extraction (SPE) procedure was required for preconcentration and sample clean-up. The separation was achieved using a C18 column (150 mm × 0.5 mm I.D, 5 µm particle size) and a mobile phase consisting of ACN : water using gradient mode, with a flow rate of 10 µl min−1. Taking advantages of the characteristics of capillary HPLC, low volume of sample and solvents were required, achieving limits of detection for the studied compounds ranged from 10.0–29.6 ng l−1 for water samples and 1.8–5.6 µg kg−1 for cucumber, using UV-detection. Recoveries studies for fortified samples, at three different concentration levels, were carried out obtaining recoveries ranging from 70.0 to 111.1% and relative standard deviations (RSDs) lower than 10.6%.
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Document Type: Research Article
Affiliations: Department of Analytical Chemistry,Faculty of Sciences, University of Granada, Avd. Fuente nueva s/nE-18071 Granada, Spain
Publication date: December 1, 2011