scholarly journals Thin-layer Chromatography–Nuclear Magnetic Resonance Spectroscopy – A Versatile Tool for Pharmaceutical and Natural Products Analysisa

2012 ◽  
Vol 66 (5) ◽  
pp. 347-349 ◽  
Author(s):  
Angelo Gössi ◽  
Uta Scherer ◽  
Götz Schlotterbeck
Planta Medica ◽  
2019 ◽  
Vol 85 (11/12) ◽  
pp. 917-924 ◽  
Author(s):  
Yanhui Ge ◽  
Xiaojia Chen ◽  
Dejan Gođevac ◽  
Paula C. P. Bueno ◽  
Luis F. Salomé Abarca ◽  
...  

AbstractIdeally, metabolomics should deal with all the metabolites that are found within cells and biological systems. The most common technologies for metabolomics include mass spectrometry, and in most cases, hyphenated to chromatographic separations (liquid chromatography- or gas chromatography-mass spectrometry) and nuclear magnetic resonance spectroscopy. However, limitations such as low sensitivity and highly congested spectra in nuclear magnetic resonance spectroscopy and relatively low signal reproducibility in mass spectrometry impede the progression of these techniques from being universal metabolomics tools. These disadvantages are more notorious in studies of certain plant secondary metabolites, such as saponins, which are difficult to analyse, but have a great biological importance in organisms. In this study, high-performance thin-layer chromatography was used as a supplementary tool for metabolomics. A method consisting of coupling 1H nuclear magnetic resonance spectroscopy and high-performance thin-layer chromatography was applied to distinguish between Ophiopogon japonicus roots that were collected from two growth locations and were of different ages. The results allowed the root samples from the two growth locations to be clearly distinguished. The difficulties encountered in the identification of the marker compounds by 1H nuclear magnetic resonance spectroscopy was overcome using high-performance thin-layer chromatography to separate and isolate the compounds. The saponins, ophiojaponin C or ophiopogonin D, were found to be marker metabolites in the root samples and proved to be greatly influenced by plant growth location, but barely by age variation. The procedure used in this study is fully described with the purpose of making a valuable contribution to the quality control of saponin-rich herbal drugs using high-performance thin-layer chromatography as a supplementary analytical tool for metabolomics research.


Molecules ◽  
2021 ◽  
Vol 26 (20) ◽  
pp. 6308
Author(s):  
Zhi-Fan Wang ◽  
Yu-Lin You ◽  
Fei-Fei Li ◽  
Wen-Ru Kong ◽  
Shu-Qi Wang

In the fields of medicine and health, traditional high-performance liquid chromatography or UV-visible spectrophotometry is generally used for substance quantification. However, over time, nuclear magnetic resonance spectroscopy (NMR) has gradually become more mature. Nuclear magnetic resonance spectroscopy has certain advantages in the quantitative analysis of substances, such as being nondestructive, having a high flux and short analysis time. Nuclear magnetic resonance spectroscopy has been included in the pharmacopoeiae of various countries. In this paper, the principle of nuclear magnetic resonance spectroscopy and the recent progress in the quantitative study of natural products by NMR are reviewed, and its application in the quantitative study of natural products is proposed. At the same time, the problems of using NMR alone to quantify natural products are summarized and corresponding suggestions are put forward.


1998 ◽  
Vol 64 (3) ◽  
pp. 890-895 ◽  
Author(s):  
Masahiro Nogawa ◽  
Hiroya Takahashi ◽  
Aya Kashiwagi ◽  
Kenji Ohshima ◽  
Hirofumi Okada ◽  
...  

ABSTRACT Chitosan-degrading activities induced by glucosamine (GlcN) orN-acetylglucosamine (GlcNAc) were found in a culture filtrate of Trichoderma reesei PC-3-7. One of the chitosan-degrading enzymes was purified to homogeneity by precipitation with ammonium sulfate followed by anion-exchange and hydrophobic-interaction chromatographies. The enzyme was monomeric, and its molecular mass was 93 kDa. The optimum pH and temperature of the enzyme were 4.0 and 50°C, respectively. The activity was stable in the pH range 6.0 to 9.0 and at a temperature below 50°C. Reaction product analysis from the viscosimetric assay and thin-layer chromatography and 1H nuclear magnetic resonance spectroscopy clearly indicated that the enzyme was an exo-type chitosanase, exo-β-d-glucosaminidase, that releases GlcN from the nonreducing end of the chitosan chain. 1H nuclear magnetic resonance spectroscopy also showed that the exo-β-d-glucosaminidase produced a β-form of GlcN, demonstrating that the enzyme is a retaining glycanase. Time-dependent liberation of the reducing sugar from partially acetylated chitosan with exo-β-d-glucosaminidase and the partially purified exo-β-d-N-acetylglucosaminidase from T. reesei PC-3-7 suggested that the exo-β-d-glucosaminidase cleaves the glycosidic link of either GlcN-β(1→4)-GlcN or GlcN-β(1→4)-GlcNAc.


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