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Determination of Total Sennosides and Sennosides A, B, and A(1) in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR

In the present work, a two-dimensional qNMR method for the determination of sennosides was established. Using band-selective HSQC and the cross correlations of the characteristic 10–10’ bonds, we quantified the total amount of the value-determining dianthranoids in five minutes, thus, rendering the...

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Autores principales: Çiçek, Serhat Sezai, Moreno Cardenas, Calisto, Girreser, Ulrich
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2022
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9656819/
https://www.ncbi.nlm.nih.gov/pubmed/36364175
http://dx.doi.org/10.3390/molecules27217349
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author Çiçek, Serhat Sezai
Moreno Cardenas, Calisto
Girreser, Ulrich
author_facet Çiçek, Serhat Sezai
Moreno Cardenas, Calisto
Girreser, Ulrich
author_sort Çiçek, Serhat Sezai
collection PubMed
description In the present work, a two-dimensional qNMR method for the determination of sennosides was established. Using band-selective HSQC and the cross correlations of the characteristic 10–10’ bonds, we quantified the total amount of the value-determining dianthranoids in five minutes, thus, rendering the method not only fast, but also specific and stability indicating. The validation of the method revealed excellent accuracy (recovery rates of 98.5 to 103%), precision (RSD values of 3.1%), and repeatability (2.2%) and demonstrated the potential of 2D qNMR in the quality control of medicinal plants. In a second method, the use of 2D qNMR for the single analysis of sennosides A, B, and A(1) was evaluated with acceptable measurement times (31 min), accuracy (93.8%), and repeatability (5.4% and 5.6%) for the two major purgatives sennoside A and B. However, the precision for sennoside B and A(1) was not satisfactory, mainly due to the low resolution of the HSQC signals of the two compounds.
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spelling pubmed-96568192022-11-15 Determination of Total Sennosides and Sennosides A, B, and A(1) in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR Çiçek, Serhat Sezai Moreno Cardenas, Calisto Girreser, Ulrich Molecules Article In the present work, a two-dimensional qNMR method for the determination of sennosides was established. Using band-selective HSQC and the cross correlations of the characteristic 10–10’ bonds, we quantified the total amount of the value-determining dianthranoids in five minutes, thus, rendering the method not only fast, but also specific and stability indicating. The validation of the method revealed excellent accuracy (recovery rates of 98.5 to 103%), precision (RSD values of 3.1%), and repeatability (2.2%) and demonstrated the potential of 2D qNMR in the quality control of medicinal plants. In a second method, the use of 2D qNMR for the single analysis of sennosides A, B, and A(1) was evaluated with acceptable measurement times (31 min), accuracy (93.8%), and repeatability (5.4% and 5.6%) for the two major purgatives sennoside A and B. However, the precision for sennoside B and A(1) was not satisfactory, mainly due to the low resolution of the HSQC signals of the two compounds. MDPI 2022-10-29 /pmc/articles/PMC9656819/ /pubmed/36364175 http://dx.doi.org/10.3390/molecules27217349 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
Çiçek, Serhat Sezai
Moreno Cardenas, Calisto
Girreser, Ulrich
Determination of Total Sennosides and Sennosides A, B, and A(1) in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR
title Determination of Total Sennosides and Sennosides A, B, and A(1) in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR
title_full Determination of Total Sennosides and Sennosides A, B, and A(1) in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR
title_fullStr Determination of Total Sennosides and Sennosides A, B, and A(1) in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR
title_full_unstemmed Determination of Total Sennosides and Sennosides A, B, and A(1) in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR
title_short Determination of Total Sennosides and Sennosides A, B, and A(1) in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR
title_sort determination of total sennosides and sennosides a, b, and a(1) in senna leaflets, pods, and tablets by two-dimensional qnmr
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9656819/
https://www.ncbi.nlm.nih.gov/pubmed/36364175
http://dx.doi.org/10.3390/molecules27217349
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