UPLC-MS/MS Analysis of Hydroxyanthracene Derivatives in Botanical Food Products and Supplements: Surveillance of the Italian Market

Hydroxyanthracene derivatives (HADs) are natural compounds that occur in several botanical species belonging to the genera <i>Aloe</i> L., <i>Cassia</i> L., <i>Rheum</i> L., <i>Frangula</i> Mill., and <i>Rhamnus</i> L. While they are widely...

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Main Authors: Mariantonietta Peloso, Alessandro Capriotti, Damiano Accurso, Elena Butovskaya, Giorgio Fedrizzi, Elisabetta Caprai
Format: Article
Language:English
Published: MDPI AG 2025-03-01
Series:Foods
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Online Access:https://www.mdpi.com/2304-8158/14/7/1229
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author Mariantonietta Peloso
Alessandro Capriotti
Damiano Accurso
Elena Butovskaya
Giorgio Fedrizzi
Elisabetta Caprai
author_facet Mariantonietta Peloso
Alessandro Capriotti
Damiano Accurso
Elena Butovskaya
Giorgio Fedrizzi
Elisabetta Caprai
author_sort Mariantonietta Peloso
collection DOAJ
description Hydroxyanthracene derivatives (HADs) are natural compounds that occur in several botanical species belonging to the genera <i>Aloe</i> L., <i>Cassia</i> L., <i>Rheum</i> L., <i>Frangula</i> Mill., and <i>Rhamnus</i> L. While they are widely used for their laxative effects, concerns persist about their potential genotoxicity and carcinogenicity. This study presents the development, validation, and application of a sensitive and rapid LC-MS/MS method to detect HAD (aloins, aloe-emodin, emodin, and danthron) levels in botanical food products and supplements. The method was validated according to criteria established by the European Union Reference Laboratory for Mycotoxins and Plant Toxins, and Regulation (EU) No 2783/2023 and was demonstrated to be fit-for-purpose. It was applied to 43 samples collected from the Italian market, including beverages, liquid and solid food supplements, herbal infusions, and jam based on aloe, senna, cassia, rhubarb, and frangula. The results revealed that 33% of the analyzed samples contained detectable HAD concentrations above the limit of quantification (LOQ = 0.5 mg/kg). The highest concentrations, up to 1352.9 mg/kg for the sum of aloin A and B, were found in solid food supplements derived from senna, cascara, rhubarb, and frangula. Aloe-emodin reached 213.4 mg/kg in a solid food supplement sample containing the same plant species, while the maximum detected concentration of emodin was 259.7 mg/kg in a senna-based supplement. No sample contained danthron. Conversely, in the majority of aloe beverage samples, HAD levels were found to be below the LOQ. In order to ensure the safety of consumers, it is essential that a more rigorous market surveillance of botanical food products is implemented, along with further toxicological studies.
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spelling doaj-art-52e9cb5d9cfd4436bf46dff9eae3f85d2025-08-20T03:08:53ZengMDPI AGFoods2304-81582025-03-01147122910.3390/foods14071229UPLC-MS/MS Analysis of Hydroxyanthracene Derivatives in Botanical Food Products and Supplements: Surveillance of the Italian MarketMariantonietta Peloso0Alessandro Capriotti1Damiano Accurso2Elena Butovskaya3Giorgio Fedrizzi4Elisabetta Caprai5National Reference Laboratory for Plant Toxins in Food, Food Chemistry Department, Istituto Zooprofilattico Sperimentale della Lombardia e dell’Emilia Romagna “Bruno Ubertini” (IZSLER), Via P. Fiorini 5, 40127 Bologna, ItalyNational Reference Laboratory for Plant Toxins in Food, Food Chemistry Department, Istituto Zooprofilattico Sperimentale della Lombardia e dell’Emilia Romagna “Bruno Ubertini” (IZSLER), Via P. Fiorini 5, 40127 Bologna, ItalyNational Reference Laboratory for Plant Toxins in Food, Food Chemistry Department, Istituto Zooprofilattico Sperimentale della Lombardia e dell’Emilia Romagna “Bruno Ubertini” (IZSLER), Via P. Fiorini 5, 40127 Bologna, ItalyFood and Feed Chemistry Department, Istituto Zooprofilattico Sperimentale della Lombardia e dell’Emilia Romagna “Bruno Ubertini” (IZSLER), Via A. Bianchi 9, 25124 Brescia, ItalyNational Reference Laboratory for Plant Toxins in Food, Food Chemistry Department, Istituto Zooprofilattico Sperimentale della Lombardia e dell’Emilia Romagna “Bruno Ubertini” (IZSLER), Via P. Fiorini 5, 40127 Bologna, ItalyNational Reference Laboratory for Plant Toxins in Food, Food Chemistry Department, Istituto Zooprofilattico Sperimentale della Lombardia e dell’Emilia Romagna “Bruno Ubertini” (IZSLER), Via P. Fiorini 5, 40127 Bologna, ItalyHydroxyanthracene derivatives (HADs) are natural compounds that occur in several botanical species belonging to the genera <i>Aloe</i> L., <i>Cassia</i> L., <i>Rheum</i> L., <i>Frangula</i> Mill., and <i>Rhamnus</i> L. While they are widely used for their laxative effects, concerns persist about their potential genotoxicity and carcinogenicity. This study presents the development, validation, and application of a sensitive and rapid LC-MS/MS method to detect HAD (aloins, aloe-emodin, emodin, and danthron) levels in botanical food products and supplements. The method was validated according to criteria established by the European Union Reference Laboratory for Mycotoxins and Plant Toxins, and Regulation (EU) No 2783/2023 and was demonstrated to be fit-for-purpose. It was applied to 43 samples collected from the Italian market, including beverages, liquid and solid food supplements, herbal infusions, and jam based on aloe, senna, cassia, rhubarb, and frangula. The results revealed that 33% of the analyzed samples contained detectable HAD concentrations above the limit of quantification (LOQ = 0.5 mg/kg). The highest concentrations, up to 1352.9 mg/kg for the sum of aloin A and B, were found in solid food supplements derived from senna, cascara, rhubarb, and frangula. Aloe-emodin reached 213.4 mg/kg in a solid food supplement sample containing the same plant species, while the maximum detected concentration of emodin was 259.7 mg/kg in a senna-based supplement. No sample contained danthron. Conversely, in the majority of aloe beverage samples, HAD levels were found to be below the LOQ. In order to ensure the safety of consumers, it is essential that a more rigorous market surveillance of botanical food products is implemented, along with further toxicological studies.https://www.mdpi.com/2304-8158/14/7/1229hydroxyanthracene derivativesLC-MS/MSvalidation<i>Aloe vera</i><i>Cassia</i><i>Rheum</i>
spellingShingle Mariantonietta Peloso
Alessandro Capriotti
Damiano Accurso
Elena Butovskaya
Giorgio Fedrizzi
Elisabetta Caprai
UPLC-MS/MS Analysis of Hydroxyanthracene Derivatives in Botanical Food Products and Supplements: Surveillance of the Italian Market
Foods
hydroxyanthracene derivatives
LC-MS/MS
validation
<i>Aloe vera</i>
<i>Cassia</i>
<i>Rheum</i>
title UPLC-MS/MS Analysis of Hydroxyanthracene Derivatives in Botanical Food Products and Supplements: Surveillance of the Italian Market
title_full UPLC-MS/MS Analysis of Hydroxyanthracene Derivatives in Botanical Food Products and Supplements: Surveillance of the Italian Market
title_fullStr UPLC-MS/MS Analysis of Hydroxyanthracene Derivatives in Botanical Food Products and Supplements: Surveillance of the Italian Market
title_full_unstemmed UPLC-MS/MS Analysis of Hydroxyanthracene Derivatives in Botanical Food Products and Supplements: Surveillance of the Italian Market
title_short UPLC-MS/MS Analysis of Hydroxyanthracene Derivatives in Botanical Food Products and Supplements: Surveillance of the Italian Market
title_sort uplc ms ms analysis of hydroxyanthracene derivatives in botanical food products and supplements surveillance of the italian market
topic hydroxyanthracene derivatives
LC-MS/MS
validation
<i>Aloe vera</i>
<i>Cassia</i>
<i>Rheum</i>
url https://www.mdpi.com/2304-8158/14/7/1229
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