24 research outputs found

    New frontiers in pharmaceutical analysis: A metabolomic approach to check batch compliance of complex products based on natural substances

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    Natural substances, particularly medicinal plants and their extracts, are still today intended as source for new Active Pharmaceutical Ingredients (APIs). Alternatively they can be validly employed to prepare medicines, food supplements or medical devices. The most adopted analytical approach used to verify quality of natural substances like medicinal plants is based still today on the traditional quantitative determination of marker compounds and/or active ingredients, besides the acquisition of a fingerprint by TLC, NIR, HPLC, GC. Here a new analytical approach based on untargeted metabolomic fingerprinting by means of Mass Spectrometry (MS) to verify the quality of grinTuss adulti syrup, a complex products based on medicinal plants, is proposed. Recently, untargeted metabolomic has been successfully applied to assess quality of natural substances, plant extracts, as well as corresponding formulated products, being the complexity a resource but not necessarily a limit. The untargeted metabolomic fingerprinting includes the monitoring of the main constituents, giving weighted relevance to the most abundant ones, but also considering minor components, that might be notable in view of an integrated \ue2\u80\u93 often synergistic \ue2\u80\u93 effect on the biological system. Two different years of production were investigated. The collected samples were analyzed by Flow Injection ElectroSpray Ionization Mass Spectrometry Analysis (FIA-ESI-MS) and a suitable data processing procedure was developed to transform the MS spectra into robust fingerprints. Multivariate Statistical Process Control (MSPC) was applied in order to obtain multivariate control charts that were validated to prove the effectiveness of the proposed method

    Experimental Evidence of the Presence of Bimolecular Caffeine/Catechin Complexes in Green Tea Extracts

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    A hypothesis on the peculiar pharmacological behavior of biologically active natural compounds is based on the occurrence of molecular interactions originating from the high complexity of the natural matrix, following the rules of supramolecular chemistry. In this context, some investigations were performed to establish unequivocally the presence of caffeine/catechin complexes in green tea extracts (GTEs). 1H NMR spectroscopy was utilized to compare profiles from GTEs with caffeine/catechin mixtures in different molar ratios, showing that peaks related to caffeine in GTEs are generally upfield shifted compared to those of free caffeine. On the other hand, ESIMS experiments performed on GTE, by means of precursor ion scan and neutral loss scan experiments, proved unequivocally the presence of caffeine/catechin complexes. Further investigations were performed by an LC-MS method operating at high-resolution conditions. The reconstructed ion chromatograms of the exact mass ions corresponding to caffeine/catechin species have been obtained, showing the presence of complexes of caffeine with gallate-type catechins. Furthermore, this last approach evidenced the presence of the same complex with different structures, consequently exhibiting different retention times. Both MSE and product ion MS/MS methods confirm the nature of caffeine/catechin complexes of the detected ions, showing the formation of protonated caffeine
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