Abstract
Phytochemical extracts are highly complex chemical mixtures. In the context of an increasing demand for phytopharmaceuticals, assessment of the phytochemical equivalence of extraction procedures is of utmost importance. Compared to routine analytical methods, comprehensive metabolite profiling has pushed forward the concept of phytochemical equivalence. In this study, an untargeted metabolomic approach was used to cross-compare four marketed extracts from Serenoa repens obtained with three different extraction processes: ethanolic, hexanic and sCO2 (supercritical carbon dioxide). Our approach involved a biphasic extraction of native compounds followed by liquid chromatography coupled to a high-resolution mass spectrometry based metabolomic workflow. Our results showed significant differences in the contents of major and minor compounds according to the extraction solvent used. The analyses showed that ethanolic extracts were supplemented in phosphoglycerides and polyphenols, hexanic extracts had higher amounts of free fatty acids and minor compounds, and sCO2 samples contained more glycerides. The discriminant model in this study could predict the extraction solvent used in commercial samples and highlighted the specific biomarkers of each process. This metabolomic survey allowed the authors to assess the phytochemical content of extracts and finished products of S. repens and unequivocally established that sCO2, hexanic and ethanolic extracts are not chemically equivalent and are therefore unlikely to be pharmacologically equivalent.
Highlights
Phytochemical extracts are complex mixtures containing dozens to thousands of compounds with a large spectrum of physico-chemical properties
The liquid chromatography-mass spectrometry (LC-MS) untargeted metabolomic approach in this study focused on native compounds and allowed the annotation of 151 features of several chemical classes
The multivariate statistical analysis in this study revealed that the extraction solvent has a direct impact on half of the compounds detected
Summary
Phytochemical extracts are complex mixtures containing dozens to thousands of compounds with a large spectrum of physico-chemical properties. The quality of herbal products can vary depending on the botanical species, geographical origin, growing and harvesting conditions and other parameters, like the choice of the solvent, extraction process and formulation [1,2]. Pre and post-extraction treatments can impact the final composition of a marketed product [3]. The assessment of the overall quality of phytochemical extracts is centered on the quantitative and/or qualitative analysis of a few biomarkers, due to a lack of purified standards and the difficulty to implement straightforward multi-target analytical methods [4]. Molecules 2019, 24, 2208 notion of chromatographic fingerprints to assess the phytochemical composition of herbal products [5]. According to the WHO, since an herbal substance or herbal preparation in its entirety is regarded as the active substance, a comprehensive determination of the stability of the constituents with known therapeutic activity should be demonstrated, by means of appropriate fingerprint chromatograms
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