Matrix-Assisted <sup>1</sup>H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>

Matrix-assisted diffusion-ordered spectroscopy (MA DOSY) technology enables efficient the virtual separation of components in a mixture according to their coefficients (D). In the current research, MA DOSY technology was applied for the analysis of a flavonoid mixture. To establish the method, five...

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Main Authors: Yulin You, Dongxiao Guo, Weiliang Cui, Zhifan Wang, Chunguo Yang, Yongqiang Lin, Shuqi Wang
Format: Article
Language:English
Published: MDPI AG 2022-11-01
Series:Separations
Subjects:
Online Access:https://www.mdpi.com/2297-8739/9/12/388
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author Yulin You
Dongxiao Guo
Weiliang Cui
Zhifan Wang
Chunguo Yang
Yongqiang Lin
Shuqi Wang
author_facet Yulin You
Dongxiao Guo
Weiliang Cui
Zhifan Wang
Chunguo Yang
Yongqiang Lin
Shuqi Wang
author_sort Yulin You
collection DOAJ
description Matrix-assisted diffusion-ordered spectroscopy (MA DOSY) technology enables efficient the virtual separation of components in a mixture according to their coefficients (D). In the current research, MA DOSY technology was applied for the analysis of a flavonoid mixture. To establish the method, five representative active flavonoid ingredients, including baicalein, baicalin, quercetin, puerarin and rutinum, were selected for the mixture model. The effects of the type and concentration of the matrix, solvent polarity, and nuclear magnetic resonance (NMR) experimental conditions on the resolution of the DOSY spectrum were investigated. It turned out that sodium dodecyl sulfate (SDS) showed the best performance in increasing the resolution of different analytes, which initially increased to the peak below the added amount of 9 mg, and decreased upon the addition of more SDS. In addition, the five flavonoids showed higher resolution in DMSO–<i>d</i><sub>6</sub> than in MeOD. Experimental parameters of DOSY, including the number of scans (NS), dummy scans (DS), and value of the FID data points (TD), were also optimized. Finally, the above optimized method was used for the qualitative analysis of the total flavonoid mixture extracted from <i>Scutellaria baicalensis</i> Georgi. A total of nine compounds were identified and confirmed by comparing them with mass spectrometry data, which further verifies the practical value of this method upon analyzing flavonoid mixtures and provides some reference significance for the follow-up research.
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spelling doaj.art-a8a4b9e3821b4ed7abd33cb093eaf7122023-11-24T17:59:15ZengMDPI AGSeparations2297-87392022-11-0191238810.3390/separations9120388Matrix-Assisted <sup>1</sup>H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>Yulin You0Dongxiao Guo1Weiliang Cui2Zhifan Wang3Chunguo Yang4Yongqiang Lin5Shuqi Wang6School of Pharmaceutical Sciences, Shandong University, 44# West Wenhua Road, Jinan 250012, ChinaShandong Institute for Food and Drug Control, Jinan 250012, ChinaShandong Institute for Food and Drug Control, Jinan 250012, ChinaSchool of Pharmaceutical Sciences, Shandong University, 44# West Wenhua Road, Jinan 250012, ChinaShandong Yifang Pharmaceutical Co., Ltd., Jinan 250012, ChinaShandong Institute for Food and Drug Control, Jinan 250012, ChinaSchool of Pharmaceutical Sciences, Shandong University, 44# West Wenhua Road, Jinan 250012, ChinaMatrix-assisted diffusion-ordered spectroscopy (MA DOSY) technology enables efficient the virtual separation of components in a mixture according to their coefficients (D). In the current research, MA DOSY technology was applied for the analysis of a flavonoid mixture. To establish the method, five representative active flavonoid ingredients, including baicalein, baicalin, quercetin, puerarin and rutinum, were selected for the mixture model. The effects of the type and concentration of the matrix, solvent polarity, and nuclear magnetic resonance (NMR) experimental conditions on the resolution of the DOSY spectrum were investigated. It turned out that sodium dodecyl sulfate (SDS) showed the best performance in increasing the resolution of different analytes, which initially increased to the peak below the added amount of 9 mg, and decreased upon the addition of more SDS. In addition, the five flavonoids showed higher resolution in DMSO–<i>d</i><sub>6</sub> than in MeOD. Experimental parameters of DOSY, including the number of scans (NS), dummy scans (DS), and value of the FID data points (TD), were also optimized. Finally, the above optimized method was used for the qualitative analysis of the total flavonoid mixture extracted from <i>Scutellaria baicalensis</i> Georgi. A total of nine compounds were identified and confirmed by comparing them with mass spectrometry data, which further verifies the practical value of this method upon analyzing flavonoid mixtures and provides some reference significance for the follow-up research.https://www.mdpi.com/2297-8739/9/12/388NMRMA-DOSYflavonoidsmixture separation
spellingShingle Yulin You
Dongxiao Guo
Weiliang Cui
Zhifan Wang
Chunguo Yang
Yongqiang Lin
Shuqi Wang
Matrix-Assisted <sup>1</sup>H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>
Separations
NMR
MA-DOSY
flavonoids
mixture separation
title Matrix-Assisted <sup>1</sup>H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>
title_full Matrix-Assisted <sup>1</sup>H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>
title_fullStr Matrix-Assisted <sup>1</sup>H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>
title_full_unstemmed Matrix-Assisted <sup>1</sup>H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>
title_short Matrix-Assisted <sup>1</sup>H DOSY Applied to Flavonoid Analysis in <i>Scutellaria baicalensis</i>
title_sort matrix assisted sup 1 sup h dosy applied to flavonoid analysis in i scutellaria baicalensis i
topic NMR
MA-DOSY
flavonoids
mixture separation
url https://www.mdpi.com/2297-8739/9/12/388
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