Optimization of a matrix solid-phase dispersion method with subsequent clean-up for the determination of ethylene
R M Garcinuño1, L Ramos, P Fernández-Hernando
1Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), 28040 Madrid, Spain.
Abstract:
A matrix solid-phase dispersion (MSPD) method with subsequent clean-up has been developed to isolate the ethylene bisdithiocarbamate (EBDC) main metabolites (ethylenethiourea, ETU, and ethylenebis [isothiocyanate] sulphide, EBIS) in almond samples. The optimized experimental set-up configuration involved 0.2 g of almond sample, washed sand as MSPD support and NaOH as defatting agent. A subsequent purification step on alumina using acetonitrile as extraction solvent was enough to remove all interferent matrix components, including the fatty material, and provide clean extracts. Quantitative analysis was performed by reversed phase liquid chromatography (RPLC) with diode-array ultraviolet absorbance (DAD UV) detector. Analytes recoveries were between 76 and 85% with relative standard deviations ranging from 3 to 12%. The low limits of quantification of 0.05 and 0.07 mg kg(-1) achieved for ETU and EBIS, respectively, make the method useful for the determination of EBDC residues on almond samples.
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