Determination of 16 Hydroxyanthracene Derivatives in Food Supplements Using LC-MS/MS: Method Development and Application

Hydroxyanthracene derivatives (HADs) are plant substances produced by a variety of plant species, including different <i>Aloe</i>, <i>Rheum</i>, and <i>Rhamnus</i> species and <i>Cassia senna.</i> These plants are often used in food supplements to impr...

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Main Authors: Svetlana V. Malysheva, Benoît Guillaume, Céline Vanhee, Julien Masquelier
Format: Article
Language:English
Published: MDPI AG 2024-11-01
Series:Toxins
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Online Access:https://www.mdpi.com/2072-6651/16/12/505
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author Svetlana V. Malysheva
Benoît Guillaume
Céline Vanhee
Julien Masquelier
author_facet Svetlana V. Malysheva
Benoît Guillaume
Céline Vanhee
Julien Masquelier
author_sort Svetlana V. Malysheva
collection DOAJ
description Hydroxyanthracene derivatives (HADs) are plant substances produced by a variety of plant species, including different <i>Aloe</i>, <i>Rheum</i>, and <i>Rhamnus</i> species and <i>Cassia senna.</i> These plants are often used in food supplements to improve bowel function. However, recently, the European Commission prohibited a number of HADs due to toxicological concerns. These HADs included aloin (aloin A and aloin B), aloe-emodin, emodin, and danthron. Most of the currently available analytical methods are restricted to the analysis of only these compounds and do not include other HADs. In this view, a multi-analyte method could be useful for both regulatory analysis and dietary intake studies. To this end, such a method, employing liquid chromatography–tandem mass spectrometry and targeting 16 different HADs, was developed and validated in this study. Limits of quantification were in the range from 0.025 mg kg<sup>−1</sup> to 1 mg kg<sup>−1</sup>. The recovery of the method was within the acceptable range of 80% to 120%, with the exception of physcion. Repeatability varied from 0.5% to 11.6%, and the range for within-laboratory reproducibility was from 3.4% to 16.3%. The expanded measurement uncertainty was below 50% for all HADs. Subsequently, 24 commercial samples of food supplements and herbal infusions sourced in Belgium were analyzed. The results indicated that although the industry put a great effort into minimizing the amount of aloin and danthron present in food supplements, more than half of the products still exceeded the maximum tolerated levels suggested for aloe-emodin and emodin.
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institution Kabale University
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spelling doaj-art-d16d145234324fdaa394643c8d7508d12024-12-27T14:56:53ZengMDPI AGToxins2072-66512024-11-01161250510.3390/toxins16120505Determination of 16 Hydroxyanthracene Derivatives in Food Supplements Using LC-MS/MS: Method Development and ApplicationSvetlana V. Malysheva0Benoît Guillaume1Céline Vanhee2Julien Masquelier3Toxins, Organic Contaminants and Additives, Physical and Chemical Health Risks, Sciensano, Leuvensesteenweg 17, 3080 Tervuren, BelgiumToxins, Organic Contaminants and Additives, Physical and Chemical Health Risks, Sciensano, Leuvensesteenweg 17, 3080 Tervuren, BelgiumMedicines and Health Products, Physical and Chemical Health Risks, Sciensano, Juliette Wytsmanstraat 14, 1050 Brussels, BelgiumToxins, Organic Contaminants and Additives, Physical and Chemical Health Risks, Sciensano, Leuvensesteenweg 17, 3080 Tervuren, BelgiumHydroxyanthracene derivatives (HADs) are plant substances produced by a variety of plant species, including different <i>Aloe</i>, <i>Rheum</i>, and <i>Rhamnus</i> species and <i>Cassia senna.</i> These plants are often used in food supplements to improve bowel function. However, recently, the European Commission prohibited a number of HADs due to toxicological concerns. These HADs included aloin (aloin A and aloin B), aloe-emodin, emodin, and danthron. Most of the currently available analytical methods are restricted to the analysis of only these compounds and do not include other HADs. In this view, a multi-analyte method could be useful for both regulatory analysis and dietary intake studies. To this end, such a method, employing liquid chromatography–tandem mass spectrometry and targeting 16 different HADs, was developed and validated in this study. Limits of quantification were in the range from 0.025 mg kg<sup>−1</sup> to 1 mg kg<sup>−1</sup>. The recovery of the method was within the acceptable range of 80% to 120%, with the exception of physcion. Repeatability varied from 0.5% to 11.6%, and the range for within-laboratory reproducibility was from 3.4% to 16.3%. The expanded measurement uncertainty was below 50% for all HADs. Subsequently, 24 commercial samples of food supplements and herbal infusions sourced in Belgium were analyzed. The results indicated that although the industry put a great effort into minimizing the amount of aloin and danthron present in food supplements, more than half of the products still exceeded the maximum tolerated levels suggested for aloe-emodin and emodin.https://www.mdpi.com/2072-6651/16/12/505hydroxyanthracene derivativesaloe-emodinemodinsennosidesLC-MS/MSfood supplements
spellingShingle Svetlana V. Malysheva
Benoît Guillaume
Céline Vanhee
Julien Masquelier
Determination of 16 Hydroxyanthracene Derivatives in Food Supplements Using LC-MS/MS: Method Development and Application
Toxins
hydroxyanthracene derivatives
aloe-emodin
emodin
sennosides
LC-MS/MS
food supplements
title Determination of 16 Hydroxyanthracene Derivatives in Food Supplements Using LC-MS/MS: Method Development and Application
title_full Determination of 16 Hydroxyanthracene Derivatives in Food Supplements Using LC-MS/MS: Method Development and Application
title_fullStr Determination of 16 Hydroxyanthracene Derivatives in Food Supplements Using LC-MS/MS: Method Development and Application
title_full_unstemmed Determination of 16 Hydroxyanthracene Derivatives in Food Supplements Using LC-MS/MS: Method Development and Application
title_short Determination of 16 Hydroxyanthracene Derivatives in Food Supplements Using LC-MS/MS: Method Development and Application
title_sort determination of 16 hydroxyanthracene derivatives in food supplements using lc ms ms method development and application
topic hydroxyanthracene derivatives
aloe-emodin
emodin
sennosides
LC-MS/MS
food supplements
url https://www.mdpi.com/2072-6651/16/12/505
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AT benoitguillaume determinationof16hydroxyanthracenederivativesinfoodsupplementsusinglcmsmsmethoddevelopmentandapplication
AT celinevanhee determinationof16hydroxyanthracenederivativesinfoodsupplementsusinglcmsmsmethoddevelopmentandapplication
AT julienmasquelier determinationof16hydroxyanthracenederivativesinfoodsupplementsusinglcmsmsmethoddevelopmentandapplication