| In present work, a sample pre-treatment method based on
a combination of homogenous liquid–liquid extraction and dispersive liquid–liquid microextraction has been proposed for the extraction of some organochlorine pesticide residues in cocoa powder
before their quantification by gas chromatography–electron capture detection. To extract the analytes, a mixture of acetonitrile and
potassium hydroxide solution is added to cocoa powder. In the
following, an appropriate amount of sodium chloride as a phase
separation agent is added and the mixture is vortexed. After centrifugation, the supernatant phase (acetonitrile containing the
extracted analytes) is separated and mixed with chloroform (as an
extraction solvent). This mixture is rapidly injected into the deionised water which its pH is 6.4. By this action, a cloudy solution is
obtained and after centrifugation, an aliquat of the sedimented
phase is removed and injected into the quantification system.
Under optimum conditions, limits of detection and quantification
of the analytes were found to be in the ranges of 0.024–0.041 and
0.081–0.138 ng g–1, respectively. The obtained extraction recoveries
varied between 50 and 89%. Also, intra – (n = 6) and inter–day
(n = 4) precisions, experiments as relative standards deviations were
less than 8.9% for the studied pesticides at different concentrations
(0.2, 1.0, 100 and 250 ng g−1, each analyte). Finally, the suggested
method was applied to determine the studied organochlorine pesticide residues in various cocoa powders gathered from groceries in
the East Azerbaijan Province, Iran. |