Chemometric study and Optimization of headspace solid-phase microextraction parameters for the determination of multiclass pesticide residues in processed cocoa from Nigeria using gas chromatography/mass spectrometry
Loading...
Date
2014-07-01
Authors
Journal Title
Journal ISSN
Volume Title
Publisher
Journal AOAC International, Official Analytical Chemists International (AOAC)
Abstract
Solid-phase microextraction (SPME) is a solventless sample preparation method that combines sample preparation, isolation, concentration, and enrichment into one step. A simple and effective method coupling headspace-SPME to GC/MS was developed for the analysis of chlorpyrifos, fenitrothion, endosulfan I, and endosulfan II pesticide residues in cocoa powder. In this study, multivariate strategy was used to determine the significance of the factors affecting the SPME of the pesticides using a Plackett-Burman design, and the significant factors were optimized using central composite design. The analytes were extracted with 100 µm polydimethylsiloxane fibers according to the factorial design matrix and desorbed into a GC/MS instrument. The developed method was applied for the analysis of a cocoa powder sample, and it exhibited good figures of merit for
the analytical methodology. Using the optimized conditions, the linearity ranged from 2.5 to 500 µg/kg (R2 > 0.99) using an internal standard calibration method, and the average recoveries were between 75 and 95%, with RSD values between 3.8 and 9.7%
Description
Keywords
Citation
41. Abdulra’uf, L. B. and Tan G. H. (2014): Chemometric study and Optimization of headspace solid-phase microextraction parameters for the determination of multiclass pesticide residues in processed cocoa from Nigeria using gas chromatography/mass spectrometry. Journal AOAC International, 97(4): 1007-1011. (Q2 ISI/Scopus cited publication). Published by Association of Official Analytical Chemists International (AOAC). Available online at https://doi.org/10.5740/jaoacint.SGEAbdulrauf