Quantitative Nuclear Magnetic Resonance and High-Performance Thin-Layer Chromatography of Cupressuflavone as a Marker for Cupressus Species

2020 ◽  
Vol 30 (4) ◽  
pp. 488-493
Author(s):  
Mohamed A. Farag ◽  
Fathalla M. Harraz ◽  
Hala M. Hammoda ◽  
Eman Shawky ◽  
Asmaa Mahana ◽  
...  
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.


1965 ◽  
Vol 43 (7) ◽  
pp. 2012-2016 ◽  
Author(s):  
Kju Hi Shin ◽  
L. Fonzes ◽  
Léo Marion

Previous work by many authors has led to the assumption that retamine might be (+)-12-hydroxysparteine. A partial synthesis of the enantiomorph of this compound has been effected by dehydration of (+)-13-hydroxylupanine and hydroboration of the product. The dehydration product consisted of two components that were separated by thin-layer chromatography and identified by the characteristics of their nuclear magnetic resonance (n.m.r.) spectra as Δ12,13-and Δ13,14-dehydrolupanine. Hydroboration of the Δ12,13-isomer gave rise to (−)-12-hydroxy-sparteine having, in thin-layer chromatography, the same Rf value as natural retamine and the same optical rotation numerically, although of opposite sign. The synthetic base had the same infrared and n.m.r. spectra as the alkaloid and the two had superimposable Debye–Scherrer patterns. Evidence is given showing the hydroxyl to be equatorial.


1968 ◽  
Vol 46 (23) ◽  
pp. 3617-3624 ◽  
Author(s):  
K. Wiesner ◽  
Z. Valenta ◽  
D. E. Orr ◽  
V. Liede ◽  
G. Kohan

The second communication of this series has shown that "pithecolobine" is a family of closely related analogues represented by the general formula 1. In the present paper a crude semiquantitative estimate of the individual components is achieved by a combination of vapor-phase chromatography and chemical degradation.The synthesis of the desoxypithecolobines 3a and 3b and their tetratosylates 11a and b11b is described. A comparison of these compounds with the corresponding "natural" mixtures by thin-layer chromatography in several systems, infrared, nuclear magnetic resonance, and mass spectrometry was found to support strongly the conclusions reached by the previous degradative work.


Author(s):  
Faiq Sulieman ◽  
Asmat Ahmad ◽  
Gires Usup ◽  
Lu Chung Kuang

Sub-minimum inhibitory concentration levels of Pseudoalteromonas ruthenica KLPp3 extract showed antibiofilm activity against Vibrio alginolyticus and Serratia marcescens. The KLPp3 crude extract was fractionated by thin layer chromatography, flash chromatography, solid phase extraction and semi-preparative high performance liquid chromatography. The pure compounds were then identified using H-nuclear magnetic resonance, C-nuclear magnetic resonance, 2D-nuclear magnetic Resonance and mass spectrometry. Nine fractions were collected from purification with two active fractions. One fractions were identified belong to the family of diketopiperazine.


Sign in / Sign up

Export Citation Format

Share Document