Chromatographic Determination of Total Selenium in Biofortified <i>Allium</i> <i>sp.</i> following Piazselenol Formation and Micro-Solid-Phase Extraction

Herein, a method based on selective piazselenol formation is applied for total selenium determination in biofortified <i>Allium</i> species. Piazselenol is formed by reacting Se(IV) with an aromatic diamine, namely 4-nitro-1,2-phenylenediamine, in acidic medium. Samples were digested in...

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Autores principales: Bogdan M. Bosca, Augustin C. Mot
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Publicado: MDPI AG 2021
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spelling oai:doaj.org-article:ad7d94e9df6740be85269ea07e601ad02021-11-11T18:40:03ZChromatographic Determination of Total Selenium in Biofortified <i>Allium</i> <i>sp.</i> following Piazselenol Formation and Micro-Solid-Phase Extraction10.3390/molecules262167301420-3049https://doaj.org/article/ad7d94e9df6740be85269ea07e601ad02021-11-01T00:00:00Zhttps://www.mdpi.com/1420-3049/26/21/6730https://doaj.org/toc/1420-3049Herein, a method based on selective piazselenol formation is applied for total selenium determination in biofortified <i>Allium</i> species. Piazselenol is formed by reacting Se(IV) with an aromatic diamine, namely 4-nitro-1,2-phenylenediamine, in acidic medium. Samples were digested in a nitric acid/hydrogen peroxide open system, followed by selenate reduction in hydrochloric acid. Reaction conditions were optimized in terms of pH, temperature, reaction time, and other auxiliary reagents for interference removal, namely, EDTA and hydroxylamine. For the extraction of the selectively formed 4-nitro-piazselenol, micro-solid-phase extraction (μSPE) was applied, and the analysis and detection of the corresponding complex was performed by HPLC coupled with DAD. An external standard calibration curve was developed (R<sup>2</sup> = 0.9994) with good sensitivity, and was used to calculate the total selenium content from several <i>Allium</i> plants material, with good intermediate precision (RSD% < 16%). The accuracy of the method was evaluated using both, a comparison with an accepted reference method from our previously published data, as well as three certified reference material with recoveries between 84–126%. The limit of detection was determined to be 0.35 μg/g (in solids) and 1.1 μg/L (in solution), while the limit of quantification was 1.07 μg/g and 3.4 μg/L (in solution). Using the proposed method, selenium content can be quickly and accurately determined in several types of samples. In addition, this study present experimental conditions for overcoming the interferences that might be encountered in selenium determination using piazselenol.Bogdan M. BoscaAugustin C. MotMDPI AGarticleselenium<i>Allium</i>piazselenolmicro-solid-phase extractionOrganic chemistryQD241-441ENMolecules, Vol 26, Iss 6730, p 6730 (2021)
institution DOAJ
collection DOAJ
language EN
topic selenium
<i>Allium</i>
piazselenol
micro-solid-phase extraction
Organic chemistry
QD241-441
spellingShingle selenium
<i>Allium</i>
piazselenol
micro-solid-phase extraction
Organic chemistry
QD241-441
Bogdan M. Bosca
Augustin C. Mot
Chromatographic Determination of Total Selenium in Biofortified <i>Allium</i> <i>sp.</i> following Piazselenol Formation and Micro-Solid-Phase Extraction
description Herein, a method based on selective piazselenol formation is applied for total selenium determination in biofortified <i>Allium</i> species. Piazselenol is formed by reacting Se(IV) with an aromatic diamine, namely 4-nitro-1,2-phenylenediamine, in acidic medium. Samples were digested in a nitric acid/hydrogen peroxide open system, followed by selenate reduction in hydrochloric acid. Reaction conditions were optimized in terms of pH, temperature, reaction time, and other auxiliary reagents for interference removal, namely, EDTA and hydroxylamine. For the extraction of the selectively formed 4-nitro-piazselenol, micro-solid-phase extraction (μSPE) was applied, and the analysis and detection of the corresponding complex was performed by HPLC coupled with DAD. An external standard calibration curve was developed (R<sup>2</sup> = 0.9994) with good sensitivity, and was used to calculate the total selenium content from several <i>Allium</i> plants material, with good intermediate precision (RSD% < 16%). The accuracy of the method was evaluated using both, a comparison with an accepted reference method from our previously published data, as well as three certified reference material with recoveries between 84–126%. The limit of detection was determined to be 0.35 μg/g (in solids) and 1.1 μg/L (in solution), while the limit of quantification was 1.07 μg/g and 3.4 μg/L (in solution). Using the proposed method, selenium content can be quickly and accurately determined in several types of samples. In addition, this study present experimental conditions for overcoming the interferences that might be encountered in selenium determination using piazselenol.
format article
author Bogdan M. Bosca
Augustin C. Mot
author_facet Bogdan M. Bosca
Augustin C. Mot
author_sort Bogdan M. Bosca
title Chromatographic Determination of Total Selenium in Biofortified <i>Allium</i> <i>sp.</i> following Piazselenol Formation and Micro-Solid-Phase Extraction
title_short Chromatographic Determination of Total Selenium in Biofortified <i>Allium</i> <i>sp.</i> following Piazselenol Formation and Micro-Solid-Phase Extraction
title_full Chromatographic Determination of Total Selenium in Biofortified <i>Allium</i> <i>sp.</i> following Piazselenol Formation and Micro-Solid-Phase Extraction
title_fullStr Chromatographic Determination of Total Selenium in Biofortified <i>Allium</i> <i>sp.</i> following Piazselenol Formation and Micro-Solid-Phase Extraction
title_full_unstemmed Chromatographic Determination of Total Selenium in Biofortified <i>Allium</i> <i>sp.</i> following Piazselenol Formation and Micro-Solid-Phase Extraction
title_sort chromatographic determination of total selenium in biofortified <i>allium</i> <i>sp.</i> following piazselenol formation and micro-solid-phase extraction
publisher MDPI AG
publishDate 2021
url https://doaj.org/article/ad7d94e9df6740be85269ea07e601ad0
work_keys_str_mv AT bogdanmbosca chromatographicdeterminationoftotalseleniuminbiofortifiedialliumiispifollowingpiazselenolformationandmicrosolidphaseextraction
AT augustincmot chromatographicdeterminationoftotalseleniuminbiofortifiedialliumiispifollowingpiazselenolformationandmicrosolidphaseextraction
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