• Analytical Science and Technology
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• v.7 no.4
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• pp.505-515
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• 1994

$^1H$ NMR spectra for monocyanide ligated ferriprotoporphyrin(hemin) complex and dicyanide coordinated hemin complex in dimethylsulfoxide(DMSO-$d_6$) solution have been recorded and analyzed. NMR spectra of hemin-cyanide complexation in DMSO-$d_6$ exhibit that the cyanide ligation to hemin is temperature-dependent. Thermodynamic parameters for the monocyanide ligated hemin to dicyanide ligated hemin are consistent with endothermic process with ${\Delta}H^{\circ}=736.6cal/mol$ and ${\Delta}S^{\circ}=16.4eu$. Detailed analysis of the anomalous deviation from Curie behavior for CN/DMSO coordinated hemin complex demonstrates the presence of a high spin character, and this weaker axial field relative to the purely low-spin dicyanide hemin complex is supposed to attribute to instantaneously ruptured iron-DMSO bond. This complex may serve as a useful model to characterize electronic/molecular structure of hemoproteins, which one of axial ligands is weak.

• Journal of the Korean Magnetic Resonance Society
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• v.6 no.2
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• pp.94-102
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• 2002

An interesting recent application of intermolecular NOE experiment is the saturation transfer difference NMR(STD-NMR) method that is useful in screening compound libraries to identify bio-active ligands. This technique also identifies the group epitopes of the bound ligand in a reversibly forming protein-ligand complex. We present here a complete relaxation and conformational exchange matrix (CORCEMA) theory (Moseley et al., J. Magn. Reson. B, 108, 243-261 (1995)) applicable for the STD-NMR experiment. Using some ideal model systems we have analyzed the factors that influence the STD intensity changes in the ligand proton NMR spectrum when the resonances from some protons on the receptor protein are saturated. These factors will be discussed and some examples of its application in some model systems will be presented. This CORCEMA theory for STD-NMR and the associated algorithm are useful in a quantitative interpretation of the STD-NMR effects, and are likely to be useful in structure-based drug design efforts. They are also useful in a quantitative characterization of protein-protein (or protein-nucleic acid) contact surfaces from an intermolecular cross-saturation NMR experiment.

• Natural Product Sciences
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• v.12 no.4
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• pp.237-240
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• 2006

Paeoniflorin, the major component of the root of Paeonia lactiflora, was quantitatively analyzed using $^1H-NMR$ spectrometry. The quantity of paeoniflorin was calculated by the ratio of the intensity of the signals (H-9, H-10, H-2', 6') to the aldehyde peak of the known amount of internal standard, 2,4,6-trihydroxybenzaldehyde. These results were compared with the conventional HPLC method. The contents of paeoniflorin in P. lactiflora, which were respectively calculated by H-9, H-10, H-2', 6' in the $^1H-NMR$ spectra and HPLC, were determined $2.60{\pm}0.07,\;2.44{\pm}0.09,\;2.77{\pm}0.12\;and\;2.46{\pm}0.16%$. The advantages of quantitative $^1H-NMR$ analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curves. Besides, it allows rapid and simple quantification for paeoniflorin with an analysis time for only 20 min without any preprocessing.

• Journal of the Korean Magnetic Resonance Society
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• v.10 no.1
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• pp.96-104
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• 2006

The gene coding for APG8a (At4g21980), a protein from Arabidopsis thaliana, is involved in the autophagy process. The protein is an interesting candidate for structure determination by NMR spectroscopy. Toward this end, APG8a has been produced recombinantly in Escherichia coli and typical NMR experiments such as $^{15}N-HSQC$, HNCA, HN(CO)CA, CBCA(CO)NH, HCCH-TOCSY, HNCO were performed. The backbone resonances, HN, N, CA, CB, and C' were sequence-specifically assigned, and the secondary structures including 3 $\alpha$ helices and $4\beta$ strands were deduced based on the assignments. Due to the intrinsic flexibility or the effect of the denaturant, the backbone resonances were not fully observed. Since the structure calculation by NMR data was not possible, the 3-dimensional model was built based on the sequence homology, and compared with the NMR results. The overall structure of the model could explain and complement the NMR derived secondary structures.

• Journal of the Korean Magnetic Resonance Society
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• v.10 no.1
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• pp.38-45
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• 2006

The NMR and MS techniques were applied to identification and quantitative analysis of oligomers in a commercialized poly (trimethylene terephthalate). Oligomers in a commercialized poly (trimethylene terephthalate) were extracted via a dissolving and reprecipitation method. Analysis of the components of the extract using NMR and MS revealed that it contained mainly cyclic oligomers with degrees of polymerization of 2, 4 and 5 (dimer, tetramer and pentamer). Trimer and cyclic oligomers with degrees of polymerization of more than 6 were not found in the extract in the present study. Quantitative analysis of dimer was performed by NMR spectroscopy.

• Journal of the Korean Chemical Society
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• v.63 no.2
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• pp.78-84
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• 2019

High-resolution $^1H$ NMR spectroscopic technique has been widely used as one of the most powerful analytical tools in food chemistry as well as to define molecular structure. The $^1H$ NMR spectra-based metabolomics has focused on classification and chemometric analysis of complex mixtures. The principal component analysis (PCA), an unsupervised clustering method and used to reduce the dimensionality of multivariate data, facilitates direct peak quantitation and pattern recognition. Using a combination of these techniques, the various green teas and black teas brewed were investigated via metabolite profiling. These teas were characterized based on the leaf size and country of cultivation, respectively.

• Journal of the Korean Magnetic Resonance Society
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• v.23 no.2
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• pp.56-60
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• 2019

Study on the structure and dynamics of molecules at the atomic level is of great significance for understanding their function and stability as well as roles for various chemico-physical and biological processes. $^{17}O$ NMR spectroscopy has appeared as an elegant technique for investigating of the physicochemical and structural properties of oxygen-containing compounds such as metal organic frameworks and nanosized oxides. This method has drawn much attention as it provides unique insights into the properties of targets based on atomistic information of local oxygen environments which is otherwise difficult to obtain using other methods. In this mini review, we introduce and discuss the recent study and developments of $^{17}O$ NMR techniques which are tailored for the investigation on the structure and dynamics of water and inorganic materials.

• Analytical Science and Technology
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• v.23 no.1
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• pp.97-101
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• 2010

(R)-N-3,5-dinitrobenzoyl (DNB) phenylglycinol derived chiral selector was used as a HPLC chiral stationary phase (CSP) for the resolution of racemic N-acylnaphthylalkylamines. In this study, determination of optical purity was performed by both chiral chromatography and NMR spectroscopy by using the (R)-phenylglycinol derived chiral selector. The data of accuracy and precision of each optical purity value are calculated from the results of NMR and HPLC experiments by comparing with true value. Average error of the NMR method was +2.2% with average RSD of 4.54%, while that of HPLC method was -3.5% with average RSD of 3.23%.

• Korean Journal of Pharmacognosy
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• v.19 no.3
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• pp.153-169
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• 1988

The combined use of the J-modulated selective INEPT and CSCM 1DNMR techniques is described for the structure elucidation of several new classes of compound including prionitin, the loureirins and larreantin, and for the regiosubstitution of the furanonaphthoquinones. Spectroscopic studies on the conformation of the cytotoxic agent savinin are also described, together with the NMR assignments and preliminary biosynthetic experiments on the antitumor antibiotic staurosporine.

• YAKHAK HOEJI
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• v.26 no.3
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• pp.139-148
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• 1982