Project type:

international,

granted by ORGANISATION FOR THE PROHIBITION OF CHEMICAL WEAPONS,

Project Account No: L/ICA/ICB/218811119

Duration:

2019 - 2021

Project Coordinator:

University of Belgrade - ICTM - National Institute of the Republic of Serbia, Department of Chemistry, Belgrade, Serbia

Participants:

University of Belgrade - ICTM - National Institute of the Republic of Serbia, Department of Chemistry, Belgrade, Serbia

University of Belgrade – Faculty of Chemistry, Serbia

Institute for Medicinal Plant Research “Dr. Josif Pančić”, Serbia

University of Bologna, Department of Pharmacology and Biotechnology, Italy

Project Manager:

Dr Dejan Gođevac, ICTM - Department of Chemistry

Number of Researchers:

11

Aim and Scope:

The scope of the project is to develop final and easy to follow protocols to unequivocally detect the fraud of specific type of herbs and dietary supplements using metabolomics approach. This approach will overcome traditional methods based on a „target list” that can often fail to detect peculiar events. Special attention will be given to the detection of chemical compounds that might be harmful for human health. This comprehensive metabolomics approach aims to protect the genuine producers and consumers from fraud by detecting, deterring and therefore preventing adulterations and counterfeits.

Specific objectives of the project are:

1.          To detect unique biomarkers of adulterants and counterfeits found in the herbs and dietary supplements.

2.         To develop NMR, GC-MS, LC-MS, or HPTLC based metabolomics platform for detection of unique biomarkers of adulterants and counterfeits found in specific herbs and dietary supplements.

3.         To disseminate project results in order to raise awareness of herbs and dietary supplements frauds.

Major Results:

a. Plant species and adulterant selected, dietary supplements selected.

The criteria for plant species selection was based on their high price and strong market demand. The first two plants selected for the further investigation were Origanum vulgare L. and Origanum onites L. Olive leaves, myrtle, sumac, cistus, and blackberry leaves determined as potential adulterants of O. vulgare L. and O. onites L. Next, chokeberry (Aronia melanocarpa (Michx.) Elliott) was also plant selected for the further investigation. Solanum nigrum, Phytolacca dodecandra, Sambucus ebulus, and Sambucus nigra determined as potential adulterants of Aronia melanocarpa.

For the selection of the most suitable dietary supplements for the investigation, special attention was given to weight loss supplements. This is according to our previous coincidental findings where synthetic chemicals with strong physiological effect and possible serious undesirable side effects were detected in the supplements declared as “natural”.

b. GC-MS, NMR, LC-MS, and HPTLC analyses performed

Oregano samples were subjected to GC-MS and ¹H NMR profiling. Chokeberry and its adulterants samples were subjected to morphological analysis and HPTLC profiling. Two dietary supplements, were analyzed by NMR methods.

c. Statistical models created

d. Biomarkers of adulterants and counterfeits identified

Pinitol was established as a biomarker of oregano adulterated with cistus.

The next biomarkers of chokeberry adulterants identified: betanin (Phytolacca dodecandra), petunidin 3-O-(p-coumaroyl)-rutinoside-5-O-glucoside (Solanum nigrum), and Cyanidin 3-O-sambubioside (Sambucus nigra).

In one dietary supplement, sibutramine a synthetic appetite suppressant which has been discontinued in many countries, has been identified. In another dietary supplement, fluoxetine, an antidepressant drug, has been identified.

Selected publications:

1. Manuela Mandrone, Lorenzo Marincich, Ilaria Chiocchio, Alessandra Petroli, Dejan Gođevac, Immacolata Maresca, Ferruccio Poli. NMR-based metabolomics for frauds detection and quality control of oregano samples. Food Control. 2021, 108141
2. Stefan Ivanović, Petar Ristivojević, Gordana Zdunić, Danilo Stojanović, Katarina Šavikin, Dejan Gođevac. Detection of Chokeberry Adulteration by HPTLC-Based Metabolomics. 2nd International UNIfood Conference, 24th-25th September 2021, University of Belgrade
3. Stefan Ivanović, Dejan Gođevac, Petar Ristivojević, Gordana Zdunić, Danilo Stojanović, Katarina Šavikin HPTLC-based metabolomics approach for the detection of chokeberry adulteration, submitted
4. Stefan Ivanović, Manuela Mandrone, Katarina Simić, Mirjana Ristić, Marina Todosijević, Boris Mandić, Dejan Gođevac. GC-MS-based metabolomics for the detection of adulteration in oregano samples. submitted

Contacts:

Dr Dejan Gođevac, ICTM - Department of Chemistry, Studentski trg 12-16, 11000 Beograd
E-mail: dejan.godjevac@ihtm.bg.ac.rs