• Journal of the Korean Magnetic Resonance Society
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• v.1 no.1
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• pp.45-58
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• 1997

Heteropoly compounds, H3PMo12O40, CsxH3-xPMo12O40, and vanadium containing heteropoly compound were characterized by Solid-state broad line 1H MAS NMR, 31P MAS NMR, and High Speed MAS 51V NMR spectroscopy of quadrupolar nuclei. The effects of calcination, dehydration, and the number of protons on the structure of heteropoly compounds were studied. The results of this study demonstrate that these Solid-state NMR techniques are very useful tools to study heteropoly compounds.

• Applied Biological Chemistry
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• v.48 no.3
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• pp.267-272
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• 2005

trans-Cinnamaldehyde, a major component of Cinnamomum cassia, was quantitatively analyzed using the $^1H-NMR$ spectrometry. Applicability of this method was confirmed through observing the variation of chemical shift in the $^1H-NMR$ spectrum of t-cinnamaldehyde and the integration value according to various sample concentrations or running temperatures. When the $^1H-NMR$ spectrometry was run for t-cinnamaldehyde (7.1429 mg/ml) at 19, 25, 30, 40 and $50^{\circ}C$, the chemical shifts of the doublet methine signal due to an aldehyde group were observed at 9.7202, 9.7184, 9.7169, 9.7142 and 9.7124 ppm, respectively, to imply that the running temperature had no significant variation in the chemical shift of the signal. The integration values of the signal were $1.37\;(19^{\circ}C),\;1.37\;(25^{\circ}C),\;1.37\;(30^{\circ}C),\;1.37(40^{\circ}C)$ and $1.37(50^{\circ}C)$, respectively, to also indicate running temperature gave no effect on the integration value. When the sample solutions with various concentrations such as 0.4464, 0.8929, 1.7857, 3.5714, 7.1429 and 14.286 mg/ml were respectively measured for the $^1H-NMR$ at $25^{\circ}C$, the chemical shifts of the aldehyde group were observed at 9.7206, 9.7201, 9.7196, 9.7192, 9.7185 and 9.7174 ppm. Even though the signal was slightly shifted to the high field in proportion to the increase of sample concentration, the alteration was not significant enough to applicate this method. The calibration curve for integration values of the doublet methine signal due to the aldehyde group vs the sample concentration was linear and showed very high regression rate ($r^2=1.0000$). Meantime, the $^1H-NMR$ spectra (7.1429 mg/ml $CDCl_3,\;25^{\circ}C$) of t-cinnamaldehyde and t-2-methoxycinnamaldehyde, another constituent of Cinnamomum cassia, showed the chemical shifts of the aldehyde group as ${\delta}_H$ 9.7174 (9.7078, 9.7270) for the former compound and ${\delta}_H$ 9.6936 (9.6839, 9.7032) for the latter one. The difference of the chemical shift between two compounds was big enough to be distinguished using the NMR spectrometer with 0.45 Hz of resolution. The contents of cinnamaldehyde in Cinnamomum cassia, which were respectively extracted with n-hexane, $CHCl_3$, and EtOAc, were determiend as 94.2 \;mg/g (0.94%), 137.6 mg/g (1.38%) and 140.1 mg/g(1.40%) t-cinnamaldehyde in each extract, respectively, by using the above method.

• Journal of the Korean Magnetic Resonance Society
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• v.15 no.1
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• pp.54-68
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• 2011

$^1H$ nuclear magnetic resonance (NMR) spectroscopy of biological samples has been proven to be an effective and nondestructive approach to probe drug toxicity within an organism. In this study, ketoprofen toxicity was investigated using $^1H$-NMR spectroscopy coupled with multivariate statistical analysis. Histopathologic test of ketoprofen-induced acute gastrointestinal damage in rats demonstrated a significant dose-dependent effect. Furthermore, principal component analysis (PCA) derived from $^1H$-NMR spectra of urinary samples showed clear separation between the vehicle-treated control and ketoprofen-treated groups. Moreover, PCA derived from endogenous metabolite concentrations through targeted profiling revealed a dose-dependent metabolic shift between the vehicle-treated control, low-dose ketoprofen-treated (10 mg/kg body weight), and high-dose ketoprofen-treated (50 mg/kg) groups coinciding with their gastric damage scores after ketoprofen administration. The resultant metabolic profiles demonstrated that the ketoprofen-induced gastric damage exhibited energy metabolism perturbations that increased urinary levels of citrate, cis-aconitate, succinate, and phosphocreatine. In addition, ketoprofen administration induced an enhancement of xenobiotic activity in fatty oxidation, which caused increase levels of N-isovalerylglycine, adipate, phenylacetylglycine, dimethylamine, betaine, hippurate, 3-indoxylsulfate, N,N-dimethylglycine, trimethyl-N-oxide, and glycine. These findings demonstrate that $^1H$-NMR-based urinary metabolic profiling can be used for noninvasive and rapid way to diagnose adverse drug effects and is suitable for explaining the possible biological pathways perturbed by nonsteroidal anti-inflammatory drug toxicity.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.46 no.3
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• pp.37-43
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• 2014

Kinetics of holocellulose hydrolysis in concentrated sulfuric acid was analyzed using $^1H$-NMR spectroscopy with different reaction time, temperature and acid concentration in secondary hydrolysis. In this work, reaction condition of secondary hydrolysis was similar to concentrated sulfuric acid process with electrodialysis or simulated moving bed chromatography process for sulfuric acid recycling. By $^1H$-NMR spectroscopy, acid hydrolyzates from higher secondary acid hydrolysis (25-35% acid concentration) was successfully analyzed without any difficulties in neutralization or adsorption of acid hydrolyzate to solid salt. Higher acid concentration, higher temperature and longer reaction time led to more cellulose for glucose conversion but accompanied with glucose to galactose isomerization, glucose to unknown compounds and degradation of glucose to organic acid via furans.

• Journal of the Korean Magnetic Resonance Society
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• v.10 no.2
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• pp.163-174
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• 2006

Luteinizing Hormone Releasing Hormone(LHRH) is a decapeptide neurotransmitter known to be regulated by metal ions in the hyperthalamus. Zn-binding LHRH complex was systhesized, and zinc-LHRH complex was studied to understand what kinds of structural modifications would be critical in the LHRH releasing mechanism. Both nonexchangeable and exchangeable $^1H-NMR$ signal assignments were accomplished by pH-dependent and COSY NMR experiments. In addition, $^1H-NMR$ chemical shift changes of a-proton and peptide NH NMR signals at different pH condition, and $^1H-NMR$ signal differences between metal free and metallo-LHRH complex was monitored. NMR signals exhibit that primary metal-binding sites are nitrogens donor of imidazole ring and Arg, and peptide oxygen of Pro-His in the sequence. Structure obtained in this study has a cyclic conformation which is similar to that of energy minimized, and exhibits a specific a-helical turn with residue numbers $(2{\sim}7)$ out of 10 amino acids.

• 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.

• Korean Journal of Microbiology
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• v.25 no.4
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• pp.304-308
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• 1987

The mode of transglycosylation reaction observed during the action of low-molecular-weight 1,4-$\beta$-D-glucan glucanohydrolase (EC 3.2.1.4) purified from Trichoderma koningii ATCC 26113 was investigated using $^{1}H-NMR $spectroscopy. The H-1 proton resonances were analysed. After reaction of the enzyme with cellotriose, the reaction products were separated by high performance liquid chromatography. H-1 resonances of the products were consisted with those of cellobiose, cellotriose and cellotitraose, respectively. Therefore it was proved that all the reaction products formed by the action of the enzyme on cellooligosaccharides, including transglycosylation products, possess only H-NMR -1,4-glycosidic linkage(s).

• Journal of the Korean Magnetic Resonance Society
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• v.13 no.1
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• pp.15-26
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• 2009

The NMR detection of methyl groups is of keen interest because they provide the long-range distance information required to establish global folds of high molecular weight proteins. Using longitudinal $^1H$ relaxation optimization, we achieve a gain in sensitivity of approximately 1.6-fold in the methyl-TROSY and its NOESY experiments for the 38 kDa protein mitogen activated protein kinase p38 in its fully protonated and $^{13}C$ and $^{15}N$ labeled state.

• Archives of Pharmacal Research
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• v.20 no.6
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• pp.652-655
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• 1997

$^{1}H-NMR$ signals of 2-cephems and 3-cephems have been assigned and the Nuclear Overhauser Effect (NOE) study of these compounds was undertaken.

• Journal of the Korean Magnetic Resonance Society
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• v.21 no.2
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• pp.67-71
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• 2017

At high temperature, the roles of $NH_4$ and $H_2O$ in $(NH_4)_2Fe(SO_4)_2{\cdot}6H_2O$ and $(NH_4)_2Zn(SO_4)_2{\cdot}6H_2O$ single crystals were investigated using a pulse NMR spectrometer. Temperature was shown to have a significant influence, causing changes in the deformation of $NH_4$ and $H_2O$. From the $^1H$ NMR and $^{14}N$ NMR spectrum, the forms of environment surrounding $^{14}N$ in $NH_4$ groups is more important than the loss of $H_2O$ groups. NMR studies indicate that $NH_4{^+}$ ions in Tutton salts play an important role in the changes of the crystal structure at high temperatures.