Nigerian Institute for Trypanosomiasis, University of Jos, University of Yaoundé
Abstract
Medicinal plants are the richest bio-resource of drugs for traditional systems of medicine, modern medicines, food supplements, pharmaceutical intermediates and chemical entities for synthetic drugs. Human African Trypanosomiasis (HAT) is a challenging and deadly disease due to its complex epidemiology and clinical presentations. This study was conducted to investigate anti-trypanosomal action of Ximenia americana root bark on Trypanosoma brucei brucei using various solvent extracts and to develop thin layer (TLC-MS) and liquid chromatography-mass spectrometric (LC-MS) profiles of the plant. Soxhlet extraction was used to obtain acetone, 70% ethanol total extracts in addition to n-hexane, dichloromethane, ethyl acetate and methanol fractions by sequential extraction. The inhibitory activity of the various extracts was compared by testing against T. b. brucei using isometamidium chloride as standard drug. The most active extract was separated by solid-phase extraction (C18 stationary phase) to obtain fractions which were profiled by TLC-MS (+ESI) and LC-MS. It was observed that anti-trypanosomal activity of acetone (16.83% yield) and 70% ethanol (18.23% yield) were comparable. However, methanol extract exhibited the highest activity with 99.18%, 97.5% and 87.50% inhibition at 3 h incubation (room temperature) using 1000 µg, 500 µg and 250 µg concentrations respectively. The activities at 1000 µg for methanol extract and isometamidium chloride were comparable with 95% CI [-1.10, 1.77]. TLC-MS and LC-MS analyses suggested gallic acid, 2,3,4,5-tetrahydroxybenzoic acid, 2ʹ,5-dimethoxyflavone, quercetin, dihydroquercetin and sesquiterpene when compared with literature database. This study presents data that could be useful in standardisation and preparation of alternative medicine in the treatment of African trypanosomiasis.
Analysis was performed by TLC/MS using the Advion expression Compact Mass Spectrometer (CMS) and Plate Express TLC Plate Reader.
Integrated Solutions for Food Authenticity, Characterization and Safety with the expression® Compact Mass Spectrometer, AVANT® (U)HPLC and SOLATION® ICP-MS
Your integrated laboratory solution for comprehensive testing of food, ingredients and natural products. Advion offers a full suite of analytical instrumentation for characterization, screening and purity determination, including:
expression® CMS – The expression® Compact Mass Spectrometer (CMS) offers the industry’s widest range of sample introduction systems, providing rapid answers with little or no sample prep in < 30 seconds.
SOLATION® ICP-MS – Provides fast, simple, multi-element analysis of toxic metals, and essential elements and minerals in a wide array of samples, including water, soil, plant material, food and raw ingredients
AVANT® HPLC & UHPLC – Advion’s range of modular high performance, liquid chromatography systems can be used standalone with UV and UV/Vis detector options, or with the expression® CMS to provide seamlessly integrated LC/CMS under the full control of Advion’s simple, intuitive software suite.
PLATE EXPRESS® TLC PLATE READER – Plate Express® provides a simple, automated means of obtaining mass spectra directly from TLC plates, combined with Advion’s expression® CMS creating a technique known as TLC/ CMS. See results in < 30 seconds at the push of a button.
Provides simple, automated MS analysis in seconds, directly from TLC plates
The Plate Express® is a device that provides a simple, automated means of obtaining mass spectra directly from TLC plates, creating a technique known as TLC/MS. Combined with Advion Interchim Scientific’s expression® compact mass spectrometer (CMS) this becomes TLC/CMS. Using this technique, chemists can quickly and confidently identify products even in complex mixtures without additional sample preparation.
Identify spots in <1 minute
Avoid the risk of overloading the mass spectrometer – TLC spots contain the ideal amount of sample for mass spectrometry
Software controlled – spectra obtained within a few mouse clicks
Simplify the process of obtaining spectra – ideal for multi-user labs
Pierre Le Pogam, Aline Pillot, Françoise Lohezic-le Devehat, Anne-Cécile Le Lamer, Béatrice Legouin, Alice Gadea, Aurélie Sauvager, Damien Ertz, Joël Boustie
Thin-layer chromatography (TLC) still enjoys widespread popularity among lichenologists as one of the fastest and simplest analytical strategies, today remaining the primary method of assessing the secondary product content of lichens. The pitfalls associated with this approach are well known as TLC leads to characterizing compounds by comparison with standards rather than properly identifying them, which might lead to erroneous assignments, accounting for the long-held interest in hyphenating TLC with dedicated identification tools. As such, commercially available TLC/Mass Spectrometry (MS) interfaces can be easily connected to any brand of mass spectrometer without adjustments. The spots of interest are extracted from the TLC plate to retrieve mass spectrometric signals within one minute, thereby ensuring accurate identification of the chromatographed substances. The results of this hyphenated strategy for lichens are presented here by 1) describing the TLC migration and direct MS analysis of single lichen metabolites of various structural classes, 2) highlighting it through the chemical profiling of crude acetone extracts of a set of lichens of known chemical composition, and finally 3) applying it to a lichen of unknown profile, Usnea trachycarpa.
The TLC/MS analysis was carried out using Advion Expression® CMS + Plate Express.
Introducing a new type of mass spectrum, available exclusively in the Advion Peak Express™ software suite: the Delta Spectrum (ΔS). The ΔS is available with the expression® compact mass spectrometer (CMS) to look beyond chemical noise and automatically detect even the smallest peaks without knowing the m/z in advance.
With the Peak Express™ software featuring ΔS, you can:
Obtain clear detection of peaks without knowing their mass
Find adducts, dimers, fragments, side-reactions and other unexpected compounds at the click of a button, in real-time or with post-processing
Highlight minor components in complex mixtures and dirty matrices
Control mass-directed purification without providing the compound mass
Acquire XIC-quality data while scanning the entire mass range, allowing Peak Express™ to tell you the m/z
Sudan Dyes are synthesized azo-dyes which are widely used to generate color in plastics, leather, fabrics, oil, waxes, etc. They are classified as Group 3 carcinogens by the International Agency for Research on Cancer (IARC) and are banned as food additives worldwide. However, in some countries these dyes are still occasionally used in order to intensify the color in products. In this note, a TLC/CMS method using expression® compact mass spectrometer (CMS) coupled with the Plate Express™ Interface is introduced for the detection of 7 Sudan dyes in a chili matrix.
The CheMS user interface simplifies the mass spectrometry experience and makes it more accessible in chemistry and biochemistry laboratories. This allows the chemist to obtain optimal data without needing to be an expert in mass spectrometry.
Available with the Advion expression® compact mass spectrometer (CMS) is a fast and easy tool that is ideal for the teaching environment — Students simply select an ionization method for effortless instrument setup at the click of a button.
Fill out the form to download the full CheMS product note now.
The analytical verification of compounds in organic syntheses is a challenging task. The sample is often directly taken out of the reaction mixture and therefore contains many impurities and matrix components. As a result, low-level sample preparation combined with a direct analysis method is highly beneficial. TLC/MS (thin layer chromatography – mass spectrometry) is such an analytical technique.
Co-authored with Merck Millipore in Darmstadt, Germany, this application note demonstrates a normal phase TLC/CMS technique for the rapid determination of 4-aminobiphenyl in its reaction mixture.
For the application note on the TLC/CMS determination of 4-aminobiphenyl in reverse phase, click here.
The analytical verification of compounds in organic syntheses is a challenging task. The sample is often directly taken out of the reaction mixture and therefore contains many impurities and matrix components. As a result, low-level sample preparation combined with a direct analysis method is highly beneficial. TLC/MS (thin layer chromatography – mass spectrometry) is such an analytical technique.
Co-authored with Merck Millipore in Darmstadt, Germany, this application note demonstrates a reverse phase TLC/CMS technique for the rapid determination of 4-aminobiphenyl in its reaction mixture.
For the application note on the TLC/CMS determination of 4-aminobiphenyl in normal phase, click here.
Plate Express™ is a device that provides a simple, automated means of obtaining mass spectra directly from TLC plates, creating a technique known as TLC/MS. Combined with Advion Interchim Scientific’s expression® Compact Mass Spectrometer (CMS) this becomes TLC/CMS. Using this technique chemists can quickly and confidently identify products even in complex mixtures without additional sample preparation.