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Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in Turnera diffusa

The quantification of low-abundance secondary metabolites in plant extracts is an analytical problem that can be addressed by different analytical platforms, the most common being those based on chromatographic methods coupled to a high-sensitivity detection system. However, in recent years nuclear...

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Autores principales: Parra-Naranjo, Aída, Delgado-Montemayor, Cecilia, Salazar-Aranda, Ricardo, Castro-Ríos, Rocío, Saucedo, Alma L., Waksman-Minsky, Noemí
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2022
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9570796/
https://www.ncbi.nlm.nih.gov/pubmed/36235131
http://dx.doi.org/10.3390/molecules27196593
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author Parra-Naranjo, Aída
Delgado-Montemayor, Cecilia
Salazar-Aranda, Ricardo
Castro-Ríos, Rocío
Saucedo, Alma L.
Waksman-Minsky, Noemí
author_facet Parra-Naranjo, Aída
Delgado-Montemayor, Cecilia
Salazar-Aranda, Ricardo
Castro-Ríos, Rocío
Saucedo, Alma L.
Waksman-Minsky, Noemí
author_sort Parra-Naranjo, Aída
collection PubMed
description The quantification of low-abundance secondary metabolites in plant extracts is an analytical problem that can be addressed by different analytical platforms, the most common being those based on chromatographic methods coupled to a high-sensitivity detection system. However, in recent years nuclear magnetic resonance (NMR) has become an analytical tool of primary choice for this type of problem because of its reliability, inherent simplicity in sample preparation, reduced analysis time, and low solvent consumption. The versatility of strategies based on quantitative NMR (qNMR), such as internal and external standards and electronic references, among others, and the need to develop validated analytical methods make it essential to compare procedures that must rigorously satisfy the analytical well-established acceptance criteria for method validation. In this work, two qNMR methods were developed for the quantification of hepatodamianol, a bioactive component of T. diffusa. The first method was based on a conventional external standard calibration, and the second one was based on the pulse length-based concentration determination (PULCON) method using the ERETIC2 module as a quantitation tool available in TopSpin software. The results show that both procedures allow the content of the analyte of interest in a complex matrix to be determined in a satisfactory way, under strict analytical criteria. In addition, ERETIC2 offers additional advantages such as a reduction in experimental time, reagent consumption, and waste generated.
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spelling pubmed-95707962022-10-17 Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in Turnera diffusa Parra-Naranjo, Aída Delgado-Montemayor, Cecilia Salazar-Aranda, Ricardo Castro-Ríos, Rocío Saucedo, Alma L. Waksman-Minsky, Noemí Molecules Article The quantification of low-abundance secondary metabolites in plant extracts is an analytical problem that can be addressed by different analytical platforms, the most common being those based on chromatographic methods coupled to a high-sensitivity detection system. However, in recent years nuclear magnetic resonance (NMR) has become an analytical tool of primary choice for this type of problem because of its reliability, inherent simplicity in sample preparation, reduced analysis time, and low solvent consumption. The versatility of strategies based on quantitative NMR (qNMR), such as internal and external standards and electronic references, among others, and the need to develop validated analytical methods make it essential to compare procedures that must rigorously satisfy the analytical well-established acceptance criteria for method validation. In this work, two qNMR methods were developed for the quantification of hepatodamianol, a bioactive component of T. diffusa. The first method was based on a conventional external standard calibration, and the second one was based on the pulse length-based concentration determination (PULCON) method using the ERETIC2 module as a quantitation tool available in TopSpin software. The results show that both procedures allow the content of the analyte of interest in a complex matrix to be determined in a satisfactory way, under strict analytical criteria. In addition, ERETIC2 offers additional advantages such as a reduction in experimental time, reagent consumption, and waste generated. MDPI 2022-10-05 /pmc/articles/PMC9570796/ /pubmed/36235131 http://dx.doi.org/10.3390/molecules27196593 Text en © 2022 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
Parra-Naranjo, Aída
Delgado-Montemayor, Cecilia
Salazar-Aranda, Ricardo
Castro-Ríos, Rocío
Saucedo, Alma L.
Waksman-Minsky, Noemí
Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in Turnera diffusa
title Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in Turnera diffusa
title_full Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in Turnera diffusa
title_fullStr Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in Turnera diffusa
title_full_unstemmed Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in Turnera diffusa
title_short Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in Turnera diffusa
title_sort two ways to achieve the same goal—two validated quantitative nmr strategies for a low-abundance natural product in standardized extracts: the case of hepatodamianol in turnera diffusa
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9570796/
https://www.ncbi.nlm.nih.gov/pubmed/36235131
http://dx.doi.org/10.3390/molecules27196593
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