LC-MS-based metabolomics for detecting adulteration in Tribulus terrestris-derived dietary supplements

The widespread usage of Tribulus terrestris dietary supplements has elicited concerns over product authenticity and possible adulteration. This research utilized an untargeted liquid chromatography-high resolution mass spectrometry (LC-HRMS) metabolomics methodology to assess the composition of T. t...

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Main Authors: Dejan Gođevac, Jovana Stanković Jeremić, Mirjana Cvetković, Katarina Simić, Ivana Sofrenić, Jovana Ljujić, Lazar Popović, Uroš Gašić, Yen-Nhi Hoang, Tao Huan, Stefan Ivanović
Format: Article
Language:English
Published: Elsevier 2025-04-01
Series:Food Chemistry: X
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Online Access:http://www.sciencedirect.com/science/article/pii/S2590157525003232
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author Dejan Gođevac
Jovana Stanković Jeremić
Mirjana Cvetković
Katarina Simić
Ivana Sofrenić
Jovana Ljujić
Lazar Popović
Uroš Gašić
Yen-Nhi Hoang
Tao Huan
Stefan Ivanović
author_facet Dejan Gođevac
Jovana Stanković Jeremić
Mirjana Cvetković
Katarina Simić
Ivana Sofrenić
Jovana Ljujić
Lazar Popović
Uroš Gašić
Yen-Nhi Hoang
Tao Huan
Stefan Ivanović
author_sort Dejan Gođevac
collection DOAJ
description The widespread usage of Tribulus terrestris dietary supplements has elicited concerns over product authenticity and possible adulteration. This research utilized an untargeted liquid chromatography-high resolution mass spectrometry (LC-HRMS) metabolomics methodology to assess the composition of T. terrestris-derived supplements. Authentic plant materials, simulated adulterated samples, and commercial products were analyzed using principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA), and a convolutional neural network tool. The presence of PDE5 inhibitors and anabolic steroids in spiked samples was confirmed. Certain commercial products included undisclosed green tea and citrus-derived chemicals, likely incorporated to amplify stimulant effects and support testosterone-enhancing claims. Additionally, spirost-4-ene-3,12-dione was recognized as an indicator of possible steroidal saponin decomposition resulting from storage or processing conditions. This study illustrates the efficacy of LC-HRMS metabolomics in detecting supplement adulteration and emphasizes the need for rigorous quality control protocols to guarantee customer safety and product integrity.
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issn 2590-1575
language English
publishDate 2025-04-01
publisher Elsevier
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series Food Chemistry: X
spelling doaj-art-cdf2c9c949fa4db29b809c2982c14f5e2025-08-20T02:31:51ZengElsevierFood Chemistry: X2590-15752025-04-012710247610.1016/j.fochx.2025.102476LC-MS-based metabolomics for detecting adulteration in Tribulus terrestris-derived dietary supplementsDejan Gođevac0Jovana Stanković Jeremić1Mirjana Cvetković2Katarina Simić3Ivana Sofrenić4Jovana Ljujić5Lazar Popović6Uroš Gašić7Yen-Nhi Hoang8Tao Huan9Stefan Ivanović10University of Belgrade, Institute of Chemistry, Technology and Metallurgy – National Institute of the Republic of Serbia, Njegoševa 12, 11000 Belgrade, Serbia; Corresponding author.University of Belgrade, Institute of Chemistry, Technology and Metallurgy – National Institute of the Republic of Serbia, Njegoševa 12, 11000 Belgrade, SerbiaUniversity of Belgrade, Institute of Chemistry, Technology and Metallurgy – National Institute of the Republic of Serbia, Njegoševa 12, 11000 Belgrade, SerbiaUniversity of Belgrade, Institute of Chemistry, Technology and Metallurgy – National Institute of the Republic of Serbia, Njegoševa 12, 11000 Belgrade, SerbiaUniversity of Belgrade – Faculty of Chemistry, Studentski trg 12-16, 11000 Belgrade, SerbiaUniversity of Belgrade – Faculty of Chemistry, Studentski trg 12-16, 11000 Belgrade, SerbiaUniversity of Belgrade – Innovation Center of Faculty of Chemistry, Studentski trg 16, 11000 Belgrade, SerbiaUniversity of Belgrade – Institute for Biological Research “Siniša Stanković” – National Institute of Republic of Serbia, Bulevar Despota Stefana 142, 11000 Belgrade, SerbiaDepartment of Chemistry, Faculty of Science, University of British Columbia, Vancouver Campus, 2036 Main Mall, Vancouver, BC V6T 1Z1, CanadaDepartment of Chemistry, Faculty of Science, University of British Columbia, Vancouver Campus, 2036 Main Mall, Vancouver, BC V6T 1Z1, CanadaUniversity of Belgrade, Institute of Chemistry, Technology and Metallurgy – National Institute of the Republic of Serbia, Njegoševa 12, 11000 Belgrade, SerbiaThe widespread usage of Tribulus terrestris dietary supplements has elicited concerns over product authenticity and possible adulteration. This research utilized an untargeted liquid chromatography-high resolution mass spectrometry (LC-HRMS) metabolomics methodology to assess the composition of T. terrestris-derived supplements. Authentic plant materials, simulated adulterated samples, and commercial products were analyzed using principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA), and a convolutional neural network tool. The presence of PDE5 inhibitors and anabolic steroids in spiked samples was confirmed. Certain commercial products included undisclosed green tea and citrus-derived chemicals, likely incorporated to amplify stimulant effects and support testosterone-enhancing claims. Additionally, spirost-4-ene-3,12-dione was recognized as an indicator of possible steroidal saponin decomposition resulting from storage or processing conditions. This study illustrates the efficacy of LC-HRMS metabolomics in detecting supplement adulteration and emphasizes the need for rigorous quality control protocols to guarantee customer safety and product integrity.http://www.sciencedirect.com/science/article/pii/S2590157525003232Tribulus terrestrisMetabolomicsLC-HRMSDietary supplementsAdulteration
spellingShingle Dejan Gođevac
Jovana Stanković Jeremić
Mirjana Cvetković
Katarina Simić
Ivana Sofrenić
Jovana Ljujić
Lazar Popović
Uroš Gašić
Yen-Nhi Hoang
Tao Huan
Stefan Ivanović
LC-MS-based metabolomics for detecting adulteration in Tribulus terrestris-derived dietary supplements
Food Chemistry: X
Tribulus terrestris
Metabolomics
LC-HRMS
Dietary supplements
Adulteration
title LC-MS-based metabolomics for detecting adulteration in Tribulus terrestris-derived dietary supplements
title_full LC-MS-based metabolomics for detecting adulteration in Tribulus terrestris-derived dietary supplements
title_fullStr LC-MS-based metabolomics for detecting adulteration in Tribulus terrestris-derived dietary supplements
title_full_unstemmed LC-MS-based metabolomics for detecting adulteration in Tribulus terrestris-derived dietary supplements
title_short LC-MS-based metabolomics for detecting adulteration in Tribulus terrestris-derived dietary supplements
title_sort lc ms based metabolomics for detecting adulteration in tribulus terrestris derived dietary supplements
topic Tribulus terrestris
Metabolomics
LC-HRMS
Dietary supplements
Adulteration
url http://www.sciencedirect.com/science/article/pii/S2590157525003232
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