A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus
Autor(a) principal: | |
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Data de Publicação: | 2016 |
Outros Autores: | , , , |
Tipo de documento: | Artigo |
Idioma: | eng |
Título da fonte: | LOCUS Repositório Institucional da UFV |
Texto Completo: | https://doi.org/10.1016/j.talanta.2016.08.032 http://www.locus.ufv.br/handle/123456789/18752 |
Resumo: | α-Bisabolol is a natural terpene produced by Eremanthus erythropappus and is widely used in cosmetics and pharmaceuticals due to its anti-inflammatory, antibacterial and antimycotic properties. Due to these applications, a control of composition and authenticity of commercial oils rich in this terpene is required, resulting in a demand for new methodologies for quality control. In this work a rapid and efficient method for quantification of α-bisabolol in the essential oil of E. erythropappus (candeia) using 1H NMR was developed, validated and compared to gas chromatography (GC) method. The quantification of α-bisabolol by 1H NMR was successfully achieved for most of the essential oil samples of E. erythropappus evaluated, except for those with a more complex composition. To circumvent this limitation a 2D NMR COSY contour map was used. This method proved to be a fast and efficient alternative, providing results with standard deviations SD<0.3%. All evaluated parameters (selectivity, linearity, accuracy/precision, repeatability, robustness and stability of analyte and internal standard in solution) gave satisfactory results. Using the 1H NMR signals at 5.36 and 5.13 ppm, the limit of detection (LOD) and limit of quantification (LOQ) were 0.26 and 2.59 mg, respectively. The results obtained by the 1H NMR method presented SD=0.59%, smaller than the value found for GC (SD=1.18%). Tukey tests have shown that the results obtained by 1H NMR and COSY methodology are similar to the obtained by the traditional GC-FID technique using external and internal standardization and normalization with 95% confidence. |
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Cerceau, Cristiane I.Barbosa, Luiz C.A.Alvarenga, Elson S.Ferreira, Antonio G.Thomasi, Sérgio S.2018-04-17T13:42:53Z2018-04-17T13:42:53Z2016-08-1000399140https://doi.org/10.1016/j.talanta.2016.08.032http://www.locus.ufv.br/handle/123456789/18752α-Bisabolol is a natural terpene produced by Eremanthus erythropappus and is widely used in cosmetics and pharmaceuticals due to its anti-inflammatory, antibacterial and antimycotic properties. Due to these applications, a control of composition and authenticity of commercial oils rich in this terpene is required, resulting in a demand for new methodologies for quality control. In this work a rapid and efficient method for quantification of α-bisabolol in the essential oil of E. erythropappus (candeia) using 1H NMR was developed, validated and compared to gas chromatography (GC) method. The quantification of α-bisabolol by 1H NMR was successfully achieved for most of the essential oil samples of E. erythropappus evaluated, except for those with a more complex composition. To circumvent this limitation a 2D NMR COSY contour map was used. This method proved to be a fast and efficient alternative, providing results with standard deviations SD<0.3%. All evaluated parameters (selectivity, linearity, accuracy/precision, repeatability, robustness and stability of analyte and internal standard in solution) gave satisfactory results. Using the 1H NMR signals at 5.36 and 5.13 ppm, the limit of detection (LOD) and limit of quantification (LOQ) were 0.26 and 2.59 mg, respectively. The results obtained by the 1H NMR method presented SD=0.59%, smaller than the value found for GC (SD=1.18%). Tukey tests have shown that the results obtained by 1H NMR and COSY methodology are similar to the obtained by the traditional GC-FID technique using external and internal standardization and normalization with 95% confidence.engTalantav. 161, p. 71-79, December 2016Elsevier B.V.info:eu-repo/semantics/openAccessqNMRCOSY1H NMRGas chromatographyEssential oilsα-BisabololA validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappusinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleapplication/pdfreponame:LOCUS Repositório Institucional da UFVinstname:Universidade Federal de Viçosa (UFV)instacron:UFVORIGINALartigo.pdfartigo.pdfTexto completoapplication/pdf1064127https://locus.ufv.br//bitstream/123456789/18752/1/artigo.pdf81bebe312fd6cfa96c285060f81f7b9fMD51LICENSElicense.txtlicense.txttext/plain; charset=utf-81748https://locus.ufv.br//bitstream/123456789/18752/2/license.txt8a4605be74aa9ea9d79846c1fba20a33MD52THUMBNAILartigo.pdf.jpgartigo.pdf.jpgIM Thumbnailimage/jpeg6504https://locus.ufv.br//bitstream/123456789/18752/3/artigo.pdf.jpg2d802c1e22cb5b127a72bf4c4bb35769MD53123456789/187522018-04-17 23:00:40.346oai:locus.ufv.br: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Repositório InstitucionalPUBhttps://www.locus.ufv.br/oai/requestfabiojreis@ufv.bropendoar:21452018-04-18T02:00:40LOCUS Repositório Institucional da UFV - Universidade Federal de Viçosa (UFV)false |
dc.title.en.fl_str_mv |
A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus |
title |
A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus |
spellingShingle |
A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus Cerceau, Cristiane I. qNMR COSY 1H NMR Gas chromatography Essential oils α-Bisabolol |
title_short |
A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus |
title_full |
A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus |
title_fullStr |
A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus |
title_full_unstemmed |
A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus |
title_sort |
A validated 1 H NMR method for quantitative analysis of α -bisabolol in essential oils of Eremanthus erythropappus |
author |
Cerceau, Cristiane I. |
author_facet |
Cerceau, Cristiane I. Barbosa, Luiz C.A. Alvarenga, Elson S. Ferreira, Antonio G. Thomasi, Sérgio S. |
author_role |
author |
author2 |
Barbosa, Luiz C.A. Alvarenga, Elson S. Ferreira, Antonio G. Thomasi, Sérgio S. |
author2_role |
author author author author |
dc.contributor.author.fl_str_mv |
Cerceau, Cristiane I. Barbosa, Luiz C.A. Alvarenga, Elson S. Ferreira, Antonio G. Thomasi, Sérgio S. |
dc.subject.pt-BR.fl_str_mv |
qNMR COSY 1H NMR Gas chromatography Essential oils α-Bisabolol |
topic |
qNMR COSY 1H NMR Gas chromatography Essential oils α-Bisabolol |
description |
α-Bisabolol is a natural terpene produced by Eremanthus erythropappus and is widely used in cosmetics and pharmaceuticals due to its anti-inflammatory, antibacterial and antimycotic properties. Due to these applications, a control of composition and authenticity of commercial oils rich in this terpene is required, resulting in a demand for new methodologies for quality control. In this work a rapid and efficient method for quantification of α-bisabolol in the essential oil of E. erythropappus (candeia) using 1H NMR was developed, validated and compared to gas chromatography (GC) method. The quantification of α-bisabolol by 1H NMR was successfully achieved for most of the essential oil samples of E. erythropappus evaluated, except for those with a more complex composition. To circumvent this limitation a 2D NMR COSY contour map was used. This method proved to be a fast and efficient alternative, providing results with standard deviations SD<0.3%. All evaluated parameters (selectivity, linearity, accuracy/precision, repeatability, robustness and stability of analyte and internal standard in solution) gave satisfactory results. Using the 1H NMR signals at 5.36 and 5.13 ppm, the limit of detection (LOD) and limit of quantification (LOQ) were 0.26 and 2.59 mg, respectively. The results obtained by the 1H NMR method presented SD=0.59%, smaller than the value found for GC (SD=1.18%). Tukey tests have shown that the results obtained by 1H NMR and COSY methodology are similar to the obtained by the traditional GC-FID technique using external and internal standardization and normalization with 95% confidence. |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-08-10 |
dc.date.accessioned.fl_str_mv |
2018-04-17T13:42:53Z |
dc.date.available.fl_str_mv |
2018-04-17T13:42:53Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/article |
format |
article |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
https://doi.org/10.1016/j.talanta.2016.08.032 http://www.locus.ufv.br/handle/123456789/18752 |
dc.identifier.issn.none.fl_str_mv |
00399140 |
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00399140 |
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https://doi.org/10.1016/j.talanta.2016.08.032 http://www.locus.ufv.br/handle/123456789/18752 |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.ispartofseries.pt-BR.fl_str_mv |
v. 161, p. 71-79, December 2016 |
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Elsevier B.V. info:eu-repo/semantics/openAccess |
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Elsevier B.V. |
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openAccess |
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Talanta |
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