Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MS

Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MS

Red yeast rice dietary supplements (RYR DS) are largely sold in Western countries for their cholesterol-lowering/regulating effect due to monacolins, mainly monacolin K (MK), which is, in fact, lovastatin, the first statin drug on the market. <sup>1</sup>H-NMR was used as an easy, rapid...

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Main Authors: Rabab Hachem, Gaëtan Assemat, Stéphane Balayssac, Nathalie Martins-Froment, Véronique Gilard, Robert Martino, Myriam Malet-Martino
Format: Article
Language:English
Published: MDPI AG 2020-01-01
Series:Molecules
Subjects:
red yeast rice
<sup>1</sup>h-nmr
uhplc-dad-ms
mass spectrometry
monacolins
Online Access:https://www.mdpi.com/1420-3049/25/2/317
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spelling doaj-bf0ef69b705541db85215f01c6b3eacc2020-11-25T03:30:25ZengMDPI AGMolecules1420-30492020-01-0125231710.3390/molecules25020317molecules25020317Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MSRabab Hachem0Gaëtan Assemat1Stéphane Balayssac2Nathalie Martins-Froment3Véronique Gilard4Robert Martino5Myriam Malet-Martino6Biomedical NMR Group, Laboratoire SPCMIB, UMR CNRS 5068, Université Paul Sabatier, 118 route de Narbonne, 31062 Toulouse CEDEX 9, FranceBiomedical NMR Group, Laboratoire SPCMIB, UMR CNRS 5068, Université Paul Sabatier, 118 route de Narbonne, 31062 Toulouse CEDEX 9, FranceBiomedical NMR Group, Laboratoire SPCMIB, UMR CNRS 5068, Université Paul Sabatier, 118 route de Narbonne, 31062 Toulouse CEDEX 9, FranceService commun de spectrométrie de masse, Institut de Chimie de Toulouse, Université Paul Sabatier, 118 route de Narbonne, 31062 Toulouse CEDEX 9, FranceBiomedical NMR Group, Laboratoire SPCMIB, UMR CNRS 5068, Université Paul Sabatier, 118 route de Narbonne, 31062 Toulouse CEDEX 9, FranceBiomedical NMR Group, Laboratoire SPCMIB, UMR CNRS 5068, Université Paul Sabatier, 118 route de Narbonne, 31062 Toulouse CEDEX 9, FranceBiomedical NMR Group, Laboratoire SPCMIB, UMR CNRS 5068, Université Paul Sabatier, 118 route de Narbonne, 31062 Toulouse CEDEX 9, FranceRed yeast rice dietary supplements (RYR DS) are largely sold in Western countries for their cholesterol-lowering/regulating effect due to monacolins, mainly monacolin K (MK), which is, in fact, lovastatin, the first statin drug on the market. <sup>1</sup>H-NMR was used as an easy, rapid and accurate method to establish the chemical profiles of 31 RYR DS and to quantify their monacolin contents. Among all the <sup>1</sup>H resonances of the monacolins found in RYR, only those of the ethylenic protons of the hexahydronaphthalenic ring at 5.84 and 5.56 ppm are suitable for quantification because they show no overlap with the matrix signals. The total content in monacolins per capsule or tablet determined in 28 DS (the content in 3 DS being below the limit of quantification of the method, &#8776; 0.25 mg per unit dose) was close to that measured by UHPLC, as shown by the good linear correlation between the two sets of values (slope 1.00, y-intercept 0.113, r<sup>2</sup> 0.986). Thirteen of the 31 RYR DS analyzed (i.e., 42%) did not provide label information on the concentration of monacolins and only nine of the 18 formulations with an indication (i.e., 50%) actually contained the declared amount of monacolins.https://www.mdpi.com/1420-3049/25/2/317red yeast rice<sup>1</sup>h-nmruhplc-dad-msmass spectrometrymonacolins
collection DOAJ
language English
format Article
sources DOAJ
author Rabab Hachem
Gaëtan Assemat
Stéphane Balayssac
Nathalie Martins-Froment
Véronique Gilard
Robert Martino
Myriam Malet-Martino
spellingShingle Rabab Hachem
Gaëtan Assemat
Stéphane Balayssac
Nathalie Martins-Froment
Véronique Gilard
Robert Martino
Myriam Malet-Martino
Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MS
Molecules
red yeast rice
<sup>1</sup>h-nmr
uhplc-dad-ms
mass spectrometry
monacolins
author_facet Rabab Hachem
Gaëtan Assemat
Stéphane Balayssac
Nathalie Martins-Froment
Véronique Gilard
Robert Martino
Myriam Malet-Martino
author_sort Rabab Hachem
title Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MS
title_short Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MS
title_full Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MS
title_fullStr Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MS
title_full_unstemmed Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by <sup>1</sup>H-NMR and UHPLC-DAD-MS
title_sort comparative chemical profiling and monacolins quantification in red yeast rice dietary supplements by <sup>1</sup>h-nmr and uhplc-dad-ms
publisher MDPI AG
series Molecules
issn 1420-3049
publishDate 2020-01-01
description Red yeast rice dietary supplements (RYR DS) are largely sold in Western countries for their cholesterol-lowering/regulating effect due to monacolins, mainly monacolin K (MK), which is, in fact, lovastatin, the first statin drug on the market. <sup>1</sup>H-NMR was used as an easy, rapid and accurate method to establish the chemical profiles of 31 RYR DS and to quantify their monacolin contents. Among all the <sup>1</sup>H resonances of the monacolins found in RYR, only those of the ethylenic protons of the hexahydronaphthalenic ring at 5.84 and 5.56 ppm are suitable for quantification because they show no overlap with the matrix signals. The total content in monacolins per capsule or tablet determined in 28 DS (the content in 3 DS being below the limit of quantification of the method, &#8776; 0.25 mg per unit dose) was close to that measured by UHPLC, as shown by the good linear correlation between the two sets of values (slope 1.00, y-intercept 0.113, r<sup>2</sup> 0.986). Thirteen of the 31 RYR DS analyzed (i.e., 42%) did not provide label information on the concentration of monacolins and only nine of the 18 formulations with an indication (i.e., 50%) actually contained the declared amount of monacolins.
topic red yeast rice
<sup>1</sup>h-nmr
uhplc-dad-ms
mass spectrometry
monacolins
url https://www.mdpi.com/1420-3049/25/2/317
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