Mass spectrometry as a versatile ancillary technique for the rapid in situ identification of lichen metabolites directly from TLC plates

2017 ◽  
Vol 49 (5) ◽  
pp. 507-520 ◽  
Author(s):  
Pierre LE POGAM ◽  
Aline PILLOT ◽  
Françoise LOHEZIC-LE DEVEHAT ◽  
Anne-Cécile LE LAMER ◽  
Béatrice LEGOUIN ◽  
...  

AbstractThin-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.

2019 ◽  
Vol 6 (1) ◽  
Author(s):  
Damien Olivier-Jimenez ◽  
Marylène Chollet-Krugler ◽  
David Rondeau ◽  
Mehdi A. Beniddir ◽  
Solenn Ferron ◽  
...  

AbstractWhile analytical techniques in natural products research massively shifted to liquid chromatography-mass spectrometry, lichen chemistry remains reliant on limited analytical methods, Thin Layer Chromatography being the gold standard. To meet the modern standards of metabolomics within lichenochemistry, we announce the publication of an open access MS/MS library with 250 metabolites, coined LDB for Lichen DataBase, providing a comprehensive coverage of lichen chemodiversity. These were donated by the Berlin Garden and Botanical Museum from the collection of Siegfried Huneck to be analyzed by LC-MS/MS. Spectra at individual collision energies were submitted to MetaboLights (https://www.ebi.ac.uk/metabolights/MTBLS999) while merged spectra were uploaded to the GNPS platform (CCMSLIB00004751209 to CCMSLIB00004751517). Technical validation was achieved by dereplicating three lichen extracts using a Molecular Networking approach, revealing the detection of eleven unique molecules that would have been missed without LDB implementation to the GNPS. From a chemist’s viewpoint, this database should help streamlining the isolation of formerly unreported metabolites. From a taxonomist perspective, the LDB offers a versatile tool for the chemical profiling of newly reported species.


The Analyst ◽  
2020 ◽  
Vol 145 (11) ◽  
pp. 3885-3891
Author(s):  
Nancy Shyrley García-Rojas ◽  
Abigail Moreno-Pedraza ◽  
Ignacio Rosas-Román ◽  
Enrique Ramírez-Chávez ◽  
Jorge Molina-Torres ◽  
...  

An open development kit for ambient ionisation enables the fast scanning and visualisation of TLC plates with high lateral resolution.


RSC Advances ◽  
2015 ◽  
Vol 5 (92) ◽  
pp. 75395-75402 ◽  
Author(s):  
Xiaoqin Zhong ◽  
Liang Qiao ◽  
Baohong Liu ◽  
Hubert H. Girault

Direct coupling of ESTASI-MS with both hydrophilic and hydrophobic TLC for ambient in situ analysis and imaging with ultralow sample consumption.


2021 ◽  
Vol 12 (4) ◽  
pp. 807-819
Author(s):  
Ajay Kumar Meena ◽  
Poorna Venktaraman ◽  
Panda P ◽  
Murali Krishna C ◽  
Kusuma Ganji ◽  
...  

Vishamusthi (Strychnos nux-vomica Linn.), a medicinal plant described as Upavisha (semi-poisonous) group of Ayurvedic Pharmacopoeia of India. Vishamusthi has widely been used and being practiced in several illness namely nervous debility, paralysis, weakness of limbs, sexual weakness, dyspepsia and etc. Ayurveda practices strictly recommend the use of Vishamusthi in therapeutics only after proper shodhana (purificatory procedure) through specific medias such as Gomutra (cow’s urine), Godugdha (cow’s milk), Goghrita (cow’s ghee), and etc. Although various shodhana procedures are recommended in Ayurvedic treatise, but updated scientific researches regarding the shodhana methods are lacking. The present study was undertaken to investigate the physicochemical and phytochemical parameters, quantitative estimation of brucine using cutting edge research tools such as high-performance thin layer chromatography (HPTLC), liquid chromatography-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS) analyses of Vishamusthi seeds before and after purification. The remarkable changes have been observed in different physicochemical parameters, HPTLC, HPLC, GC-MS and LC-MS chromatographic profiling before and after shodhana process of Vishamusthi seeds. Quantitative HPLC studies revealed that the process of shodhana resulted in depletion of toxic brucine (chief poisonous constituent of Vishamusthi seeds) reduced to 79.66% in chloroform extract and 64.54% in ethanol extract after shodhana process.


2020 ◽  
pp. 205-210
Author(s):  
Digambar Nabhu Mokat ◽  
Sarika Daulatrao Torawane ◽  
Yogesh Chandrakant Suryawanshi

In the present investigation chemical constituents of Cyathocline purpurea (Buch.-Ham. ex D.Don) Kuntze and Blumea lacera (Burm.f.) DC. (Family-Compositae) were studied by using gas chromatography coupled with mass spectrometry (GC/MS). These two weeds are small  herbs and well known for its potent medicinal properties. Total 17 and 27 compounds were identified from C. purpurea and B. lacera respectively. The major constituents in both the extracts were pentadecanoic acid, 14-methyl-, methyl ester (30.56 %), cis-phytol (21.26 %), α- cadinol (7.87 %), γ-cadinene (7.13 %), neophytadiene (3.81 %) and α-cubebene (1.82 %). GC/MS analysis revealed the presence of various bioactive compounds such as fatty acids, sesquiterpenoids, phenols, etc. in the acetone extracts of both the plants. The identified compounds have various biological activities.


2020 ◽  
Author(s):  
Feifei Jia ◽  
Jie Wang ◽  
Yanyan Zhang ◽  
Qun Luo ◽  
Luyu Qi ◽  
...  

<p></p><p><i>In situ</i> visualization of proteins of interest at single cell level is attractive in cell biology, molecular biology and biomedicine, which usually involves photon, electron or X-ray based imaging methods. Herein, we report an optics-free strategy that images a specific protein in single cells by time of flight-secondary ion mass spectrometry (ToF-SIMS) following genetic incorporation of fluorine-containing unnatural amino acids as a chemical tag into the protein via genetic code expansion technique. The method was developed and validated by imaging GFP in E. coli and human HeLa cancer cells, and then utilized to visualize the distribution of chemotaxis protein CheA in E. coli cells and the interaction between high mobility group box 1 protein and cisplatin damaged DNA in HeLa cells. The present work highlights the power of ToF-SIMS imaging combined with genetically encoded chemical tags for <i>in situ </i>visualization of proteins of interest as well as the interactions between proteins and drugs or drug damaged DNA in single cells.</p><p></p>


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