Direct determination of methyl parathion insecticide in rice samples by headspace solid-phase microextraction-gas chromatography-mass spectrometry

BACKGROUND The organophosphorus insecticides, especially those based on methyl parathion as active principle, have been used extensively in the protection of rice in Maranhão State, in the north‐east of Brazil. This paper describes the optimisation of a solid‐phase microextraction (SPME) procedure i...

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Bibliographic Details
Published in:Pest management science 2015-11, Vol.71 (11), p.1497-1502
Main Authors: da Silva, Darlan Ferreira, Paiva Silva, Francisco Eduardo, Silva, Fernanda Gabrielle S, Nunes, Gilvanda Silva, Badea, Mihaela
Format: Article
Language:English
Subjects:
Cholinesterase Inhibitors - analysis
Chromatography
Correlation coefficient
Extraction processes
Gas chromatography
Gas Chromatography-Mass Spectrometry - methods
GC/MS
Green chemistry
Insecticides
Insecticides - analysis
Mass spectrometry
Methyl parathion
Methyl Parathion - analysis
Organophosphorus compounds
Organophosphorus pesticides
Oryza - chemistry
Parathion
Pesticide Residues - analysis
Rice
Solid Phase Microextraction - methods
solid-phase microextraction
Solids
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Summary:BACKGROUND The organophosphorus insecticides, especially those based on methyl parathion as active principle, have been used extensively in the protection of rice in Maranhão State, in the north‐east of Brazil. This paper describes the optimisation of a solid‐phase microextraction (SPME) procedure in confined atmosphere (headspace, HS) for the determination of methyl parathion in rice organic samples by gas chromatography with mass spectrometry detection (GC/MS). RESULTS The proposed HS‐SPME‐GC/MS method has been shown to be appropriate for direct analysis of the insecticide in polished rice, with satisfactory results for the following parameters: linearity (correlation coefficient 0.9985), sensitivity (LOD and LOQ of 0.026 and 0.078 µg kg−1 respectively), precision (coefficients of variation between 6.1 and 22.4%) and accuracy (recoveries varying from 73.2 to 90.0%). Although the efficiency of the proposed GC/MS does not differ statistically (P < 0.05) from the conventional GC/NPD method, given its low cost, speed and also the fact that a minimum volume of toxic effluent is generated, this method can be considered an on‐line procedure based on green chemistry. CONCLUSIONS Thus, the analytical methodology satisfies the minimum requirements for control of residues of such insecticides in rice samples destined for human consumption. © 2014 Society of Chemical Industry
ISSN:1526-498X
1526-4998
DOI:10.1002/ps.3953