Chemometric study and optimization of heads pace solid-phase microextraction parameters for the determination of multiclass pesticide residues in processed cocoa from Nigeria using gas chromatography/mass spectrometry
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, endosu...
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| Main Authors: | , |
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| Format: | Conference or Workshop Item |
| Language: | en |
| Published: |
2014
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| Subjects: | |
| Online Access: | http://eprints.um.edu.my/11418/1/0001.pdf http://eprints.um.edu.my/11418/ |
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| Summary: | 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 " 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 pm 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 pg/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%. |
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