Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant Materials

Products based on plants containing hydroxyanthracene derivatives (HADs)—such as <i>Rheum</i>, <i>Cassia</i>, and <i>Aloe</i> species—are widely used in food supplements or nutraceuticals due to their laxative effects. A more restricted control of HAD contents in...

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Main Authors: Francesca Loschi, Marta Faggian, Stefania Sut, Irene Ferrarese, Erica Maccari, Gregorio Peron, Stefano Dall’Acqua
Format: Article
Language:English
Published: MDPI AG 2022-03-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/27/6/1932
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author Francesca Loschi
Marta Faggian
Stefania Sut
Irene Ferrarese
Erica Maccari
Gregorio Peron
Stefano Dall’Acqua
author_facet Francesca Loschi
Marta Faggian
Stefania Sut
Irene Ferrarese
Erica Maccari
Gregorio Peron
Stefano Dall’Acqua
author_sort Francesca Loschi
collection DOAJ
description Products based on plants containing hydroxyanthracene derivatives (HADs)—such as <i>Rheum</i>, <i>Cassia</i>, and <i>Aloe</i> species—are widely used in food supplements or nutraceuticals due to their laxative effects. A more restricted control of HAD contents in food supplements has been implemented by EU Regulation 2021/468, in order to increase the safety of these preparations. Due to their toxicity, aloin A, aloin B, aloe emodin, emodin, and the synthetic derivative danthron have been listed as prohibited substances in food supplements, being tolerated in amounts < 1 mg kg<sup>−1</sup> in marketed products. In this work, we report the development of a sensitive and fast LC–DAD–MS-based procedure for the determination of these five compounds in food supplements and plant materials or extracts. The entire procedure includes a simple sample preparation step, where target analytes are concentrated by means of solvent extraction and evaporative concentration (solid samples), or by lyophilisation (liquid samples). The average LOQ of 0.10 mg/L, LOD of 0.03 mg/L, accuracy, and precision with CVs below 12.72 were obtained for the studied analytes. This method is suitable for assessing the compliance of commercial products and raw materials with EU Regulation 2021/468. Furthermore, the proposed method can represent a starting point for the development of a unique and standardised analytical approach for the determination of other HADs under the attention of EU authorities.
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spelling doaj.art-dd172414fa7348f592e8f4a2d6bd4e4d2023-11-30T21:43:27ZengMDPI AGMolecules1420-30492022-03-01276193210.3390/molecules27061932Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant MaterialsFrancesca Loschi0Marta Faggian1Stefania Sut2Irene Ferrarese3Erica Maccari4Gregorio Peron5Stefano Dall’Acqua6Department of Pharmaceutical and Pharmacological Sciences, University of Padova, Via Marzolo 5, 35131 Padova, ItalyUnired srl, Via Niccolo’ Tommaseo 69, 35131 Padova, ItalyDepartment of Pharmaceutical and Pharmacological Sciences, University of Padova, Via Marzolo 5, 35131 Padova, ItalyDepartment of Pharmaceutical and Pharmacological Sciences, University of Padova, Via Marzolo 5, 35131 Padova, ItalyDepartment of Pharmaceutical and Pharmacological Sciences, University of Padova, Via Marzolo 5, 35131 Padova, ItalyDepartment of Pharmaceutical and Pharmacological Sciences, University of Padova, Via Marzolo 5, 35131 Padova, ItalyDepartment of Pharmaceutical and Pharmacological Sciences, University of Padova, Via Marzolo 5, 35131 Padova, ItalyProducts based on plants containing hydroxyanthracene derivatives (HADs)—such as <i>Rheum</i>, <i>Cassia</i>, and <i>Aloe</i> species—are widely used in food supplements or nutraceuticals due to their laxative effects. A more restricted control of HAD contents in food supplements has been implemented by EU Regulation 2021/468, in order to increase the safety of these preparations. Due to their toxicity, aloin A, aloin B, aloe emodin, emodin, and the synthetic derivative danthron have been listed as prohibited substances in food supplements, being tolerated in amounts < 1 mg kg<sup>−1</sup> in marketed products. In this work, we report the development of a sensitive and fast LC–DAD–MS-based procedure for the determination of these five compounds in food supplements and plant materials or extracts. The entire procedure includes a simple sample preparation step, where target analytes are concentrated by means of solvent extraction and evaporative concentration (solid samples), or by lyophilisation (liquid samples). The average LOQ of 0.10 mg/L, LOD of 0.03 mg/L, accuracy, and precision with CVs below 12.72 were obtained for the studied analytes. This method is suitable for assessing the compliance of commercial products and raw materials with EU Regulation 2021/468. Furthermore, the proposed method can represent a starting point for the development of a unique and standardised analytical approach for the determination of other HADs under the attention of EU authorities.https://www.mdpi.com/1420-3049/27/6/1932hydroxyanthracene derivativesLC–DAD–MSfood supplementsbotanicals
spellingShingle Francesca Loschi
Marta Faggian
Stefania Sut
Irene Ferrarese
Erica Maccari
Gregorio Peron
Stefano Dall’Acqua
Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant Materials
Molecules
hydroxyanthracene derivatives
LC–DAD–MS
food supplements
botanicals
title Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant Materials
title_full Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant Materials
title_fullStr Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant Materials
title_full_unstemmed Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant Materials
title_short Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant Materials
title_sort development of an lc dad ms based method for the analysis of hydroxyanthracene derivatives in food supplements and plant materials
topic hydroxyanthracene derivatives
LC–DAD–MS
food supplements
botanicals
url https://www.mdpi.com/1420-3049/27/6/1932
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