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Low ng/1-level determination of twenty N-methylcarbamate pesticides and twelve of their polar metabolites in surface water via off-line solid-phase extraction and high-performance liquid chromatography with post-column reaction and fluorescence detection


Low ng/1-level determination of twenty N-methylcarbamate pesticides and twelve of their polar metabolites in surface water via off-line solid-phase extraction and high-performance liquid chromatography with post-column reaction and fluorescence detection



Journal of Chromatography 623(2): 265-276



ISSN/ISBN: 0021-9673

DOI: 10.1016/0021-9673(92)80366-3

Reversed-phase high-performance liquid chromatography (HPLC) was used for the determination of twenty parent N-methylcarbamate pesticides and twelve major metabolites in surface water. A 50-ml water sample was passed through a disposable solid-phase extraction cartridge, packed with 500 mg of low-carbon C-18-bonded slica (C-18/OH, 40 mu-m particle size), which selectively retained polar compounds. The preconcentrated analytes were eluted with acetonitrile, reconstituted in 1 ml of water and 100 mu-l were injected into the HPLC system. The carbamates were separated via a water-methanol-acetonitrile gradient. Detection was performed via postcolumn hydrolysis on a solid-phase (anion-exchange) catalyst, derivatization of the methylamine formed with o-phthalaldehyde-2-mercaptoethanol and fluorescence detection of the isoindole derivative. The detection limits for surface water were between 20 and 30 ng/l. Recoveries were determined for thirteen carbamates and ten metabolites at the 0.1 and 1 mu-g/l level and generally ranged from 76 to 106% with relative standard deviations (R.S.D.s) fo0.5-8.5%. Only the sulphoxide metabolite of ethiofencarb and thiofanox had lower recoveries and correspondingly higher R.S.D.s.

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Accession: 008976029

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