NMR analysis of budding yeast metabolomics: a rapid method for sample preparation

2015 ◽  
Vol 11 (2) ◽  
pp. 379-383 ◽  
Author(s):  
C. Airoldi ◽  
F. Tripodi ◽  
C. Guzzi ◽  
R. Nicastro ◽  
P. Coccetti
Keyword(s):  
Nmr Spectroscopy ◽  
Sample Preparation ◽  
Rapid Method ◽  
Budding Yeast ◽  
Yeast Cells ◽  
Intracellular Metabolite ◽  
Nmr Analysis ◽  
H Nmr ◽  
Metabolite Extraction

We present a rapid and reproducible protocol for intracellular metabolite extraction from yeast cells analyzed by1H-NMR spectroscopy.

Circular Dichroism and Conformational Analysis of Diastereomeric Bicamphors

2000 ◽  
Vol 65 (4) ◽  
pp. 477-489 ◽  
Author(s):  
Stefan E. Boiadjiev ◽  
David A. Lightner
Keyword(s):  
Nmr Spectroscopy ◽  
Conformational Analysis ◽  
Molecular Mechanics ◽  
Spectral Data ◽  
Relative Orientation ◽  
Nmr Analysis ◽  
Molecular Mechanics Calculations ◽  
H Nmr ◽  
The Third ◽  
Carbonyl Chromophores

Stereospecific syntheses afforded endo,endo- (1) and exo,exo- (2) bicamphors, while the third possible diastereomeric exo,endo-bicamphor (3) originated from nonselective camphor radical dimerization. The stereochemistry of bicamphor linkage was confirmed by 1H NMR analysis. Chiroptical and ultraviolet spectral data are presented for the three diastereomers 1-3 to show interchromophoric interaction. Conformational analysis to evaluate the relative orientation of each pair of carbonyl chromophores was accomplished by 1H NMR spectroscopy and molecular mechanics calculations.

Use of a laboratory robot for repetitive solution NMR sample preparation

1993 ◽  
Vol 71 (2) ◽  
pp. 275-279
Author(s):  
Michael A. Jeannot ◽  
R. Stephen Reid
Keyword(s):  
Sample Preparation ◽  
Solution Nmr ◽  
Nmr Analysis ◽  
Acid Base ◽  
H Nmr ◽  
Ligand System ◽  
Base Study ◽  
Nmr Sample Preparation ◽  
Nmr Signals

Observing ligand 1H NMR signals while conditions (e.g., analytical concentrations, pH) are changed in an aqueous metal–proton–ligand system is one of the most potent methods of elucidating the precise details of speciation in such systems. Typically this is performed by changing the conditions in a solution reservoir, while withdrawing a sample for NMR analysis at each stage. However, such sample preparation is tedious and time-consuming. We report here studies, using a Mitsubishi RM-101 laboratory robot, of the feasibility of completely automating such a procedure. A simple acid–base study is used to evaluate performance.

Characterization of technical lignins by NMR spectroscopy: optimization of functional group analysis by 31P NMR spectroscopy

Holzforschung ◽  
2015 ◽  
Vol 69 (6) ◽  
pp. 807-814 ◽  
Author(s):  
Philipp Korntner ◽  
Ivan Sumerskii ◽  
Markus Bacher ◽  
Thomas Rosenau ◽  
Antje Potthast
Keyword(s):  
Nmr Spectroscopy ◽  
Analytical Data ◽  
Group Analysis ◽  
Hydroxyl Group ◽  
Solution Technique ◽  
31P Nmr Spectroscopy ◽  
Nmr Analysis ◽  
H Nmr ◽  
Functional Group Analysis ◽  
First Time

Abstract31P nuclear magnetic resonance (NMR) based on the derivatization reagent 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane is a common approach for the hydroxyl group determination of lignins, but the results are sometimes less reproducible compared to other methods. In the present work, common pitfalls in31P NMR analysis of kraft lignin (KL) and lignosulfonates (LS) are addressed and the results are compared to those obtained by1H NMR spectroscopy. Several experimental parameters are revisited in terms of the reliability of the obtained data, such as the choice of relaxation delay, internal standards, and the best solution technique for the31P NMR analysis of LS. For the first time,31P NMR data of LS are presented based on a new dissolution protocol. The analytical data of a set of lignins consisting of three KLs, one LS, and one milled wood lignin are presented based on the optimized31P NMR approach.

scholarly journals 1H NMR Study of the Enantioselective Binding ofΛ- andΔ-[Ru(bpy)2(m-bpy-GHK)]Cl2to the Deoxynucleotide Duplex d(5'-C1G2C3G4A5A6T7T8C9G10C11G12-3')2

2005 ◽  
Vol 3 (1-2) ◽  
pp. 109-117 ◽  
Author(s):  
A. Myari ◽  
N. Hadjiliadis ◽  
A. Garoufis
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
Minor Groove ◽  
Major Groove ◽  
Nmr Analysis ◽  
Groove Binding ◽  
H Nmr ◽  
Nmr Study ◽  
Oligonucleotide Duplex ◽  
Diastereomeric Complexes

The interaction of the diastereomeric complexes Λ- andΔ-[Ru(bpy)2(m-GHK)]Cl2, (GHK = glycine-histidine-lysine) to the deoxynucleotide duplex d(5'-CGCGAATTCGCG-3')2was studied by means of1H NMR spectroscopy. The diastereomers interact with the oligonucleotide duplex differently. TheΔ-[Ru(bpy)2(m-GHK)]Cl2is characterized by major groove binding close to the central part of the oligonucleotide, with both the peptide and the bipyridine ligand of the complex involved in the binding. TheΛ-[Ru(bpy)2(m-bpy-GHK)]Cl2binds loosely, approaching the helix from the minor groove. The NMR analysis shows that the peptide (GHK) binding has a determinative role in the interactions of both diastereomers with the oligonucleotide.

scholarly journals Remarkable functions of sn-3 hydroxy and phosphocholine groups in 1,2-diacyl-sn-glycerolipids to induce clockwise (+)-helicity around the 1,2-diacyl moiety: Evidence from conformation analysis by 1H NMR spectroscopy

2017 ◽  
Vol 13 ◽  
pp. 1999-2009 ◽  
Author(s):  
Yoshihiro Nishida ◽  
Mengfei Yuan ◽  
Kazuo Fukuda ◽  
Kaito Fujisawa ◽  
Hirofumi Dohi ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Cell Membrane ◽  
1H Nmr Spectroscopy ◽  
Conformational Property ◽  
Nmr Analysis ◽  
Conformation Analysis ◽  
Polar Solvents ◽  
H Nmr ◽  
Head Groups ◽  
Conformational Properties

Cell-membrane glycerolipids exhibit a common structural backbone of asymmetric 1,2-diacyl-sn-glycerol bearing polar head groups in the sn-3 position. In this study, the possible effects of sn-3 head groups on the helical conformational property around the 1,2-diacyl moiety in the solution state were examined. 1H NMR Karplus relation studies were carried out using a series of 1,2-dipalmitoyl-sn-glycerols bearing different sn-3 substituents (namely palmitoyl, benzyl, hydrogen, and phosphates). The 1H NMR analysis indicated that the helical property around the 1,2-diacyl moiety is considerably affected by these sn-3 substituents. The sn-3 hydroxy group induced a unique helical property, which was considerably dependent on the solvents used. In CDCl3 solution, three staggered conformers, namely gt(+), gg(−) and tg, were randomized, while in more polar solvents, the gt(+) conformer with (+)-helicity was amplified at the expense of gg(−) and tg conformers. The sn-3 phosphocholine in phosphatidylcholine exhibited a greater effect on the gt(+) conformer, which was independent of the solvents used. From the 1H NMR analysis, the helical conformational properties around the 1,2-diacyl moiety conformed to a simple empirical rule, which permitted the proposal of a conformational diagram for 1,2-dipalmitoyl-sn-glycerols in the solution states.

Conformational study on ribonucleoside O-phosphonylmethyl derivatives by 1H NMR spectroscopy

1985 ◽  
Vol 50 (8) ◽  
pp. 1899-1905 ◽  
Author(s):  
Milena Masojídková ◽  
Jaroslav Zajíček ◽  
Miloš Buděšínský ◽  
Ivan Rosenberg ◽  
Antonín Holý
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Conformational Study ◽  
H Nmr ◽  
Conformational Properties

Conformational properties of ribonucleoside 5'-O-phosphonylmethyl derivatives have been determined by 1H NMR spectroscopy and compared with those of natural nucleosides and 5'-nucleotides.

Synthesis and Structure Assignment of 2-(4-Methoxybenzyl)cyclohexyl β-D-Glucopyranoside Enantiomers

2006 ◽  
Vol 71 (10) ◽  
pp. 1470-1483 ◽  
Author(s):  
David Šaman ◽  
Pavel Kratina ◽  
Jitka Moravcová ◽  
Martina Wimmerová ◽  
Zdeněk Wimmer
Keyword(s):  
Analytical Data ◽  
Chiral Hplc ◽  
Nmr Analysis ◽  
Target Structure ◽  
Enantiomerically Pure ◽  
Whole Cells ◽  
H Nmr ◽  
Structure Assignment ◽  
Related Compounds ◽  
C Nmr

Glucosylation of the cis- and trans-isomers of 2-(4-methoxybenzyl)cyclohexan-1-ol (1a/1b, 2a/2b, 1a or 2a) was performed to prepare the corresponding alkyl β-D-glucopyranosides, mainly to get analytical data of pure enantiomers of the glucosides (3a-6b), required for subsequent investigations of related compounds with biological activity. One of the employed modifications of the Koenigs-Knorr synthesis resulted in achieving 85-95% yields of pure β-anomers 3a/3b, 4a/4b, 3a or 4a of protected intermediates, with several promoters and toluene as solvent, yielding finally the deprotected products 5a/5b, 6a/6b, 5a or 6a as pure β-anomers. To obtain enantiomerically pure β-anomers of the target structure (3a, 4a, 5a and 6a) for unambiguous structure assignment, an enzymic reduction of 2-(4-methoxybenzyl)cyclohexan-1-one by Saccharomyces cerevisiae whole cells was performed to get (1S,2S)- and (1S,2R)-enantiomers (1a and 2a) of 2-(4-methoxybenzyl)cyclohexan-1-ol. The opposite enantiomers of alkyl β-D-glucopyranosides (5b and 6b) were obtained by separation of the diastereoisomeric mixtures 5a/5b and 6a/6b by chiral HPLC. All stereoisomers of the products (3a-6b) were subjected to a detailed 1H NMR and 13C NMR analysis.

Monitoring the encapsulation of chlorin e6 derivatives into polymer carriers by NMR spectroscopy

2019 ◽  
Vol 23 (11n12) ◽  
pp. 1576-1586 ◽  
Author(s):  
Sara Pfister ◽  
Luca Sauser ◽  
Ilche Gjuroski ◽  
Julien Furrer ◽  
Martina Vermathen
Keyword(s):  
Relaxation Time ◽  
Nmr Spectroscopy ◽  
Core Region ◽  
Chlorin E6 ◽  
Polypropylene Glycol ◽  
Polymer Carriers ◽  
H Nmr ◽  
Line Shape Analysis ◽  
Dynamic Methods ◽  
Derivatives Of

The encapsulation of five derivatives of chlorin e6 with different hydrophobicity and aggregation properties into a series of five poloxamer-type triblock copolymer micelles (BCMs) with varying numbers of polyethylene and polypropylene glycol (PEG, PPG) units was monitored using 1H NMR spectroscopy. NMR chemical shift and line shape analysis, as well as dynamic methods including diffusion ordered spectroscopy (DOSY) and T1 and T2 relaxation time measurements of the chlorin and the polymer resonances, proved useful to assess the chlorin–BCM compatibility. The poloxamers had high capability to break up aggregates formed by chlorins up to intermediate hydrophobicity. Physically entrapped chlorins were always localized in the BCM core region. The loading capacity correlated with chlorin polarity for all poloxamers among which those with the lowest number of PPG units were most efficient. DOSY data revealed that relatively weakly aggregating chlorins partition between the aqueous bulk and micellar environment whereas more hydrophobic chlorins are well retained in the BCM core region, rendering these systems more stable. T1 and T2 relaxation time measurements indicated that motional freedom in the BCM core region contributes to encapsulation efficiency. The BCM corona dynamics were rather insensitive towards chlorin entrapment except for the poloxamers with short PEG chains. The presented data demonstrate that 1H NMR spectroscopy is a powerful complementary tool for probing the compatibility of porphyrinic compounds with polymeric carriers such as poloxamer BCMs, which is a prerequisite in the development of stable and highly efficient drug delivery systems suitable for medical applications like photodynamic therapy of tumors.

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