Optimization of focused microwave-assisted extraction of DDT and derivatives from soil samples

Citation
O. Zuloaga et al., Optimization of focused microwave-assisted extraction of DDT and derivatives from soil samples, HRC-J HIGH, 23(12), 2000, pp. 681-687
Citations number
17
Categorie Soggetti
Spectroscopy /Instrumentation/Analytical Sciences
Journal title
HRC-JOURNAL OF HIGH RESOLUTION CHROMATOGRAPHY
ISSN journal
09356304 → ACNP
Volume
23
Issue
12
Year of publication
2000
Pages
681 - 687
Database
ISI
SICI code
0935-6304(200012)23:12<681:OOFMEO>2.0.ZU;2-R
Abstract
Optimization of focused microwave (FMW)-assisted extraction of 4,4'-DDE, 4, 4'-DDD, and 4,4'-DDT from soil samples was carried out using central compos ite designs. All the extracts were analyzed with GC/MS and some of them als o with GC/AED using columns of different polarities for each of the techniq ues, The extraction of the analytes was carried out in two ways: with aceti c acid as microwave radiation absorbent solvent and n-decane to concentrate the analytes and with reagent water and iso-octane as solvents. In the fir st case, the influence of the extraction temperature, the extraction time, and the addition of sodium chloride were studied and the optimum conditions for the extraction of 1 g of soil with 5 mL of acetic acid and 2 mL of n-d ecane were 1.30 mol L-1 sodium chloride at 98 degreesC for 9.3 min. In the second case, the temperature was kept constant (94 degreesC) and the influe nce of the concentration of sodium chloride and the extraction time were st udied. The optimum conditions were 5 mL of a 2.0 mol L-1 sodium chloride to gether with 2 mL of iso-octane for 15 min, The recoveries obtained by water -FMW extraction were significantly lower than those obtained by the acetic acid-FMW procedure. These last recoveries were in good agreement with those obtained by closed microwave assisted-extraction with acetone-n-hexane as solvent.