%0 Generic %D 2022 %T Multidimensional Fingerprint Development for the Detection of Tribulus terrestris in Plant Food Supplements %A Surbhi Ranjan %A Sano-Magnifique Dusingizimana %A Tanika Van Mulders %A Eric Deconinck %A Erwin Adams %K Fingerprints %K plant food supplements %K Tribulus terrestris %X

Tribulus terrestris is a popular Ayurvedic herb with potency enhancing properties. According
to the Belgian Royal Decree of 1997, Tribulus is a regulated plant when used in plant food
supplements. The dangers of self-medication and toxicity of such plant supplements is
heightened by the ease with which they can be purchased from various illegal channels,
necessitating an efficient screening approach.
This study aims to develop a multidimensional approach using chromatographic fingerprinting
at different wavelengths for identification of Tribulus terrestris in plant food supplements. A
specific, selective and fast fingerprinting method for Tribulus (reference material obtained from
the American Herbal Pharmacopoeia) was developed using ultra high performance liquid
chromatography coupled with a diode array detector. Next, a correlation analysis comparing
the wavelengths was performed and 5 orthogonal wavelengths were selected. The developed
method was tested for specificity in different triturations (1/20, 1/15, 1/10, 1/5 and 1/2). These
were prepared using 10 blank matrices and lactose. In most triturations, Tribulus could visually
be detected from concentration 1/10 onwards, by comparing the fingerprints with the reference
plant.
A market study of a total of 20 samples (with potency enhancement as indication) seized by
the Belgian Federal Agency for Medicines and Health Products (FAMHP) was carried out.
Visual inspection was conducted to detect the presence of Tribulus in the real samples. This
was done by overlaying the sample chromatograms with the reference plant and visually
comparing the fingerprints. So, out of 20 samples, 11 samples were suspected to be positive,
when analyzed at the 5 wavelengths, 254 nm and with the combined fingerprint. The multi and
combined wavelengths approach provides a characteristic and specific fingerprint with more
information at different wavelengths than only 254 nm, which is useful for visual inspection. In
a second step, mass spectrometric (MS) measurements using a time of flight analyzer were
performed. This was done in order to further confirm the presence of Tribulus in suspected
samples. After obtaining MS fingerprints, the exact mass of the main peaks (peaks with the
highest absorbance in the reference) were compared. It was concluded that out of 11 samples,
9 can be suspected to be positive for Tribulus terrestris. As future prospects, steps are being
taken to combine chromatographic fingerprinting and chemometrics in order to use these
multidimensional data and extract maximum information with the intention to create binary
models for faster screening of plant food supplements.

%B Drug Analysis %I Drug Analysis %C Mons, Belgium %8 13/09/2022 %G eng %N BSPS, UMons, ULB