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:	Maria Suely Siqueira Ferraz, Lêda Rita D’Antonino Faroni, Fernanda Fernandes Heleno, Adalberto Hipólito de Sousa, Lucas Henrique Figueiredo Prates, Alessandra Aparecida Zinato Rodrigues
Formato:	article
Lenguaje:	EN
Publicado:	MDPI AG 2021
Materias:	<i>Vigna unguiculata</i> <i>Piper hispidinervum</i> essential oil stored products bioinsecticides sample preparation Organic chemistry QD241-441
Acceso en línea:	https://doaj.org/article/7a3d284040fa4e23b97319fad090e5b3
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spelling	oai:doaj.org-article:7a3d284040fa4e23b97319fad090e5b32021-11-25T18:28:25ZMethod Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography10.3390/molecules262269141420-3049https://doaj.org/article/7a3d284040fa4e23b97319fad090e5b32021-11-01T00:00:00Zhttps://www.mdpi.com/1420-3049/26/22/6914https://doaj.org/toc/1420-3049Bioinsecticides 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 <i>Piper hispidinervum</i> 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<sup>−1</sup>, respectively and the determination coefficient (R<sup>2</sup>) 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<sup>−1</sup> (contact) and from 2.16 to 0.12 µg kg <sup>−1</sup> (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.Maria Suely Siqueira FerrazLêda Rita D’Antonino FaroniFernanda Fernandes HelenoAdalberto Hipólito de SousaLucas Henrique Figueiredo PratesAlessandra Aparecida Zinato RodriguesMDPI AGarticle<i>Vigna unguiculata</i><i>Piper hispidinervum</i>essential oilstored productsbioinsecticidessample preparationOrganic chemistryQD241-441ENMolecules, Vol 26, Iss 6914, p 6914 (2021)
institution	DOAJ
collection	DOAJ
language	EN
topic	<i>Vigna unguiculata</i> <i>Piper hispidinervum</i> essential oil stored products bioinsecticides sample preparation Organic chemistry QD241-441
spellingShingle	<i>Vigna unguiculata</i> <i>Piper hispidinervum</i> essential oil stored products bioinsecticides sample preparation Organic chemistry QD241-441 Maria Suely Siqueira Ferraz Lêda Rita D’Antonino Faroni Fernanda Fernandes Heleno Adalberto Hipólito de Sousa Lucas Henrique Figueiredo Prates Alessandra Aparecida Zinato Rodrigues Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography
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 <i>Piper hispidinervum</i> 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<sup>−1</sup>, respectively and the determination coefficient (R<sup>2</sup>) 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<sup>−1</sup> (contact) and from 2.16 to 0.12 µg kg <sup>−1</sup> (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.
format	article
author	Maria Suely Siqueira Ferraz Lêda Rita D’Antonino Faroni Fernanda Fernandes Heleno Adalberto Hipólito de Sousa Lucas Henrique Figueiredo Prates Alessandra Aparecida Zinato Rodrigues
author_facet	Maria Suely Siqueira Ferraz Lêda Rita D’Antonino Faroni Fernanda Fernandes Heleno Adalberto Hipólito de Sousa Lucas Henrique Figueiredo Prates Alessandra Aparecida Zinato Rodrigues
author_sort	Maria Suely Siqueira Ferraz
title	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_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_sort	method validation and evaluation of safrole persistence in cowpea beans using headspace solid-phase microextraction and gas chromatography
publisher	MDPI AG
publishDate	2021
url	https://doaj.org/article/7a3d284040fa4e23b97319fad090e5b3
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Method Validation and Evaluation of Safrole Persistence in Cowpea Beans Using Headspace Solid-Phase Microextraction and Gas Chromatography

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