Multiresidue method for determination of 20 organochlorine pesticide residues in fruits and vegetables using modified QuEChERS and GC-ECD/GC-MSD

Wittayanan W., . and Chaimongkol T., . and Jongmevasna W., . Multiresidue method for determination of 20 organochlorine pesticide residues in fruits and vegetables using modified QuEChERS and GC-ECD/GC-MSD. pp. 2340-2346. ISSN 2231-7546

A rapid multiresidue method has been developed for the analysis of 20 organochlorine pesticides (OCs) in fruits and vegetables. The method is based on a modified QuEChERS procedure employing acetonitrile for extraction and partition. Dispersive solid-phase extraction (dSPE) containing primary and secondary amine (PSA) and graphitized carbon black (GCB) was used for cleans-up. Analytical determinations of the 20 OCs were carried out by gas chromatography using electron capture detector (GC-ECD) and confirmed by mass spectrometry detector (GCMSD). Recovery studies were performed at 0.05 0.15 and 1.5 mg kg- fortification levels and the results of validation parameters were acceptable (accuracy ranged from 61.2 to 117.6 precision expressed as RSD were less than 20 and measurement uncertainty was lower than 50). The correlation coefficients (r ) obtained for linearity of working range test were higher than 0.995 showing that the method is applicable to routine sample. The limit of detection (LOD) and the limit of quantitation (LOQ) for the OCs tested in apple and lettuce were 0.02 and 0.05 mg kg-respectively. The developed method was applied to determine OCs in imported fruits and local vegetables. No residual OCs was detected in any vegetable sample. However detectable pesticides residues were found in 0.4 (3 apple samples) of the fruit samples. All of the positive samples were contaminated with endosulfan sulfate which is endosulfan metabolite. None of the samples had contamination higher than the maximum residue limit (MRL) set by Codex.

Full text available from: Official URL: http://www.ifrj.upm.edu.my/24%20(06)%202017/(8).pd...

Abstract

A rapid multiresidue method has been developed for the analysis of 20 organochlorine pesticides (OCs) in fruits and vegetables. The method is based on a modified QuEChERS procedure employing acetonitrile for extraction and partition. Dispersive solid-phase extraction (dSPE) containing primary and secondary amine (PSA) and graphitized carbon black (GCB) was used for cleans-up. Analytical determinations of the 20 OCs were carried out by gas chromatography using electron capture detector (GC-ECD) and confirmed by mass spectrometry detector (GCMSD). Recovery studies were performed at 0.05 0.15 and 1.5 mg kg- fortification levels and the results of validation parameters were acceptable (accuracy ranged from 61.2 to 117.6 precision expressed as RSD were less than 20 and measurement uncertainty was lower than 50). The correlation coefficients (r ) obtained for linearity of working range test were higher than 0.995 showing that the method is applicable to routine sample. The limit of detection (LOD) and the limit of quantitation (LOQ) for the OCs tested in apple and lettuce were 0.02 and 0.05 mg kg-respectively. The developed method was applied to determine OCs in imported fruits and local vegetables. No residual OCs was detected in any vegetable sample. However detectable pesticides residues were found in 0.4 (3 apple samples) of the fruit samples. All of the positive samples were contaminated with endosulfan sulfate which is endosulfan metabolite. None of the samples had contamination higher than the maximum residue limit (MRL) set by Codex.

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Item Type:	Article
AGROVOC Term:	Fruits
AGROVOC Term:	Vegetables
AGROVOC Term:	Organochlorine compounds
AGROVOC Term:	Extraction
AGROVOC Term:	Carbon black
AGROVOC Term:	Acetone
AGROVOC Term:	Apples
AGROVOC Term:	Lettuces
AGROVOC Term:	Acetic acid
AGROVOC Term:	Identification
Depositing User:	Ms. Suzila Mohamad Kasim
Last Modified:	24 Apr 2025 06:28
URI:	http://webagris.upm.edu.my/id/eprint/23880

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