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Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography

Bioinsecticides are regarded as important alternatives for controlling agricultural pests. However, few studies have determined the persistence of these compounds in stored grains. This study aimed at optimizing and validating a fast and effective method for extraction and quantification of residues...

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Autores principales: Ferraz, Maria Suely Siqueira, Faroni, Lêda Rita D’Antonino, Heleno, Fernanda Fernandes, de Sousa, Adalberto Hipólito, Prates, Lucas Henrique Figueiredo, Rodrigues, Alessandra Aparecida Zinato
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2021
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8618816/
https://www.ncbi.nlm.nih.gov/pubmed/34834007
http://dx.doi.org/10.3390/molecules26226914
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author Ferraz, Maria Suely Siqueira
Faroni, Lêda Rita D’Antonino
Heleno, Fernanda Fernandes
de Sousa, Adalberto Hipólito
Prates, Lucas Henrique Figueiredo
Rodrigues, Alessandra Aparecida Zinato
author_facet Ferraz, Maria Suely Siqueira
Faroni, Lêda Rita D’Antonino
Heleno, Fernanda Fernandes
de Sousa, Adalberto Hipólito
Prates, Lucas Henrique Figueiredo
Rodrigues, Alessandra Aparecida Zinato
author_sort Ferraz, Maria Suely Siqueira
collection PubMed
description Bioinsecticides are regarded as important alternatives for controlling agricultural pests. However, few studies have determined the persistence of these compounds in stored grains. This study aimed at optimizing and validating a fast and effective method for extraction and quantification of residues of safrole (the main component of Piper hispidinervum essential oil) in cowpea beans. It also sought to assess the persistence of this substance in the grains treated by contact and fumigation. The proposed method used headspace solid-phase microextraction (HS-SPME) and gas chromatography with a flame ionization detector (GC/FID). Factors such as temperature, extraction time and type of fiber were assessed to maximize the performance of the extraction technique. The performance of the method was appraised via the parameters selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy. The LOD and LOQ of safrole were 0.0057 and 0.019 μg kg(−1), respectively and the determination coefficient (R(2)) was >0.99. The relative recovery ranged from 99.26 to 104.85, with a coefficient of variation <15%. The validated method was applied to assess the persistence of safrole residue in grains, where concentrations ranged from 1.095 to 0.052 µg kg(−1) (contact) and from 2.16 to 0.12 µg kg (−1) (fumigation). The levels measured up from the fifth day represented less than 1% of the initial concentration, proving that safrole have low persistence in cowpea beans, thus being safe for bioinsecticide use. Thus, this work is relevant not only for the extraction method developed, but also for the possible use of a natural insecticide in pest management in stored grains.
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spelling pubmed-86188162021-11-27 Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography Ferraz, Maria Suely Siqueira Faroni, Lêda Rita D’Antonino Heleno, Fernanda Fernandes de Sousa, Adalberto Hipólito Prates, Lucas Henrique Figueiredo Rodrigues, Alessandra Aparecida Zinato Molecules Article Bioinsecticides are regarded as important alternatives for controlling agricultural pests. However, few studies have determined the persistence of these compounds in stored grains. This study aimed at optimizing and validating a fast and effective method for extraction and quantification of residues of safrole (the main component of Piper hispidinervum essential oil) in cowpea beans. It also sought to assess the persistence of this substance in the grains treated by contact and fumigation. The proposed method used headspace solid-phase microextraction (HS-SPME) and gas chromatography with a flame ionization detector (GC/FID). Factors such as temperature, extraction time and type of fiber were assessed to maximize the performance of the extraction technique. The performance of the method was appraised via the parameters selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy. The LOD and LOQ of safrole were 0.0057 and 0.019 μg kg(−1), respectively and the determination coefficient (R(2)) was >0.99. The relative recovery ranged from 99.26 to 104.85, with a coefficient of variation <15%. The validated method was applied to assess the persistence of safrole residue in grains, where concentrations ranged from 1.095 to 0.052 µg kg(−1) (contact) and from 2.16 to 0.12 µg kg (−1) (fumigation). The levels measured up from the fifth day represented less than 1% of the initial concentration, proving that safrole have low persistence in cowpea beans, thus being safe for bioinsecticide use. Thus, this work is relevant not only for the extraction method developed, but also for the possible use of a natural insecticide in pest management in stored grains. MDPI 2021-11-16 /pmc/articles/PMC8618816/ /pubmed/34834007 http://dx.doi.org/10.3390/molecules26226914 Text en © 2021 by the authors. https://creativecommons.org/licenses/by/4.0/Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Ferraz, Maria Suely Siqueira
Faroni, Lêda Rita D’Antonino
Heleno, Fernanda Fernandes
de Sousa, Adalberto Hipólito
Prates, Lucas Henrique Figueiredo
Rodrigues, Alessandra Aparecida Zinato
Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography
title Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography
title_full Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography
title_fullStr Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography
title_full_unstemmed Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography
title_short Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography
title_sort method validation and evaluation of safrole persistence in cowpea beans using headspace solid-phase microextraction and gas chromatography
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8618816/
https://www.ncbi.nlm.nih.gov/pubmed/34834007
http://dx.doi.org/10.3390/molecules26226914
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