• Journal of the Korean Magnetic Resonance Society
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• v.17 no.1
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• pp.40-46
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• 2013

For a case study of suspected paraquat intoxication, we developed a simple and rapid method of $^1H$ qNMR to determine the mili-molar amount of paraquat in postmortem blood samples. There were no interfering signals from endogenous compounds in the chemical shift of paraquat and diquat (internal standard). The amount of sample used ranged from 0.25 mM to 10.0 mM. Diquat, which has similar physicochemical properties with paraquat, was chosen as an internal standard. The NMR experimental conditions, relaxation delay time and CPMG spin-echo pulse sequence were optimized. The developed method was validated in terms of specificity, accuracy, precision, matrix effect, recovery, limit of detection (LOD), and low limit of quantification (LLOQ). The proposed qNMR method provided a simple and rapid assay for the identification and quantification of the quaternary ammonium herbicide, "paraquat" in postmortem blood samples. This method was tested by using the blood from the heart of a man who was intoxicated with paraquat. In this particular case, the level of paraquat was 1.07 mM in the blood. For the determination of quaternary ammonium herbicides, qNMR could also be used to provide a better understanding of the currently available techniques.

• Korean Journal of Agricultural Science
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• v.35 no.1
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• pp.11-17
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• 2008

This study was conducted to isolate polyacetylenes from the Acanthopanax senticosus and to identify the chemical structure of the polyacetylenes by UV, IR, $^1H$-NMR and $^{13}C$-NMR. One of the liposoluble materials was extracted with petroleum ether. Polyacetylene compounds were collected through solvent fractionation at silica gel column chromatograph. The HPLC was used for the semi-preparative separation IR spectra of fraction 5 showed triple bonds at $2256cm^{-1}$ and double bond at $1654cm^{-1}$, respectively, $^1H$-NMR spectra of Fraction 5 showed the double bond at 5.35-5.48 ppm. Triple bond at 64.0. 71.2, 74.2, 80.2 ppm and double bond at 121.89, 133.0 ppm were observed in the $^{13}C$-NMR spectra.

• Journal of Ginseng Research
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• v.40 no.3
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• pp.245-250
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• 2016

Background: Ginsenosides are the major effective ingredients responsible for the pharmacological effects of ginseng. Malonyl ginsenosides are natural ginsenosides that contain a malonyl group attached to a glucose unit of the corresponding neutral ginsenosides. Methods: Medium-pressure liquid chromatography and semipreparative high-performance liquid chromatography were used to isolate purified compounds and their structures determined by extensive one-dimensional- and two-dimensional nuclear magnetic resonance (NMR) experiments. Results: A new saponin, namely malonyl-ginsenoside Re, was isolated from the fresh flower buds of Panax ginseng, along with malonyl-ginsenosides Rb1, Rb2, Rc, Rd. Some assignments for previously published $^1H$- and $^{13}C$-NMR spectra were found to be inaccurate. Conclusion: This study reports the complete NMR assignment of malonyl-ginsenoside Re, $Rb_1$, $Rb_2$, Rc, and Rd for the first time.

• Food Science of Animal Resources
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• v.41 no.2
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• pp.312-323
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• 2021

The purpose of this study was to use 1H nuclear magnetic resonance (1H NMR) to quantify taste-active and bioactive compounds in chicken breasts and thighs from Korean native chicken (KNC) [newly developed KNCs (KNC-A, -C, and -D) and commercial KNC-H] and white-semi broiler (WSB) used in Samgye. Further, each breed was differentiated using multivariate analyses, including a machine learning algorithm designed to use metabolic information from each type of chicken obtained using 1H-13C heteronuclear single quantum coherence (2D NMR). Breast meat from KNC-D chickens were superior to those of conventional KNC-H and WSB chickens in terms of both taste-active and bioactive compounds. In the multivariate analysis, meat portions (breast and thigh) and chicken breeds (KNCs and WSB) could be clearly distinguished based on the outcomes of the principal component analysis and partial least square-discriminant analysis (R2=0.945; Q2=0.901). Based on this, we determined the receiver operating characteristic (ROC) curve for each of these components. AUC analysis identified 10 features which could be consistently applied to distinguish between all KNCs and WSB chickens in both breast (0.988) and thigh (1.000) meat without error. Here, both 1H NMR and 2D NMR could successfully quantify various target metabolites which could be used to distinguish between different chicken breeds based on their metabolic profile.

• Proceedings of the Korean Society of Applied Pharmacology
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• 1994.04a
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• pp.267-267
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• 1994

In order to obtain insight into the mechanism by which DNA containing a thymine photo-dimer is recognized by the excision repair enzyme, T$_4$ endonuclease V, we have taken NMR study of this protein and its complex with oligonucleotides. The conformations of five different DNA duplexes DNA I : d(GCGGATGGCG).d(CGCCTACCGC), DNA II d(GCGGTTGGCG) .d(CGCCAACCGC), DNA III : d(GCGGT ^ TGGCG) .d(CGCCAACCGC), DNA IV d(GCGGGCGGCG).d(CGCCCGCCGC) and DNA V d(GCGGCCGGCG) . d(CGCCGGCCGC) were studied by $^1$H NMR. The NMR spectra of these five DNA duplexes in the absence of the enzyme clearly show that the formation of a thymine dimer within the DNA induces only a minor distortion in the structure, and that the overall structure of B type DNA is retained. The photo-dimer formation is found to cause a large change in chemical shifts at the GC7 base pair, which is located at the 3'-side of the thymine dimer, accompanied by the major conformational change at the thymine dimer site. The binding of a mutant T$_4$ endonuclease V (E23Q), which is unable to digest DNA containing a thymine dimer, to the DNA duplex d(GCGGT ^ TGGCG)ㆍd(CGCCAACCGC) causes a large down-field shift in the imino proton resonance of GC7. Therefore, this position is thought to be either the crucial point of the interaction wi th T$_4$ endonuclease V, or the si to of a conformational change in the DNA caused by the binding of T$_4$ endonuclease V. Usually, it is very difficult to assign NMR peaks in DNA * protein complex because of severe peak overlaps. In order to overcome these peak overlaps, we used a method of deuterium incorporation.

• Bulletin of the Korean Chemical Society
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• v.27 no.9
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• pp.1397-1400
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• 2006

A detailed spectroscopic study ($^1H$ NMR, COSY, ROESY) of complexation of venlafaxine hydrochloride (VEN) with $\beta$-cyclodextrin ($\beta$--CD) was carried out in solution. The stoichiometry of the complex was determined to be 1 : 1 and penetration of aromatic ring into $\beta$-Cyclodextrin cavity was confirmed from primary rim side, with the help of ROESY spectral data. The structure of the venlafaxine hydrochloride-$\beta$-CD complex has been proposed. The association constant was determined to be 234 $M^{-1}$.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.14 no.11
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• pp.941-946
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• 2001

The fundamental study on HTV silicone for insulation material has been performed. In order to estimate the chemical behavior of siloxane under high voltage, H-NMR, GPC and vinyl contents measurement were used. As an experimental results, after high voltage stress, the molecular weight of siloxane are increased, the vinyl contents of siloxane are decreased. The dielectric strength of vinyl group containing siloxane was lower than only methyl containing siloxane.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.19 no.12
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• pp.814-824
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• 2018

This study was conducted to investigate VFA, monosaccharides and metabolites in rumen fluid according to feeding methods. Three castrated Hanwoo steers were used to the $3{\times}3$ Latin square design, 10 day for the diet adaptation period. VFA and monosaccharides which were not detected by HPLC and HPAEC however, those were detected by $^1H-NMR$. Among the metabolites measured by $^1H-NMR$ carbohydrate metabolites, pyruvate was detected only in the rumen fluid before feeding and succinate was detected before and after feeding rumen fluid. In amino acid total 9 metabolites were detected. In lipid metabolites, ethylene glycol was significantly higher (P<0.05) in before feeding Con group. In aliphatic acylic metabolite, trimethylamine N-oxide was no significant difference observed compare to Con group. In this study, many metabolites were observed in the rumen fluid by $^1H-NMR$, and it confirmed that rumen metabolic products were changed by feeding methods.

• Journal of the Mineralogical Society of Korea
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• v.24 no.4
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• pp.301-312
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• 2011

The study on the atomic structure of iron-bearing silicate glasses has significant geological implications for both diverse igneous processes on Earth surface and ultra-low velocity zones at the core-mantle boundary. Here, we report experimental results on the effect of iron content on the atomic structure in iron-bearing alkali silicate glasses ($Na_2O-Fe_2O_3-SiO_2$ glasses, up to 16.07 wt% $Fe_2O_3$) using $^{29}Si$ and $^{17}O$ solid-state NMR spectroscopy. $^{29}Si$ spin-lattice ($T_1$) relaxation time for the glasses decreases with increasing iron content due to an enhanced interaction between nuclear spin and unpaired electron in iron. $^{29}Si$ MAS NMR spectra for the glasses show a decrease in signal intensity and an increase in peak width with increasing iron content. However, the heterogeneous peak broa-dening in $^{29}Si$ MAS NMR spectra suggests the heterogeneous distribution of $Q^n$ species around iron in iron-bearing silicate glasses. While nonbridging oxygen ($Na-O-Si$) and bridging oxygen (Si-O-Si) peaks are partially resolved in $^{17}O$ MAS NMR spectrum for iron-free silicate glass, it is difficult to distinguish the oxygen clusters in iron-bearing silicate glass. The Lorentzian peak shape for $^{29}Si$ and $^{17}O$ MAS NMR spectra may reflect life-time broadening due to spin-electron interaction. These results demonstrate that solid-state NMR can be an effective probe of the detailed structure in iron-bearing silicate glasses.

• Journal of the Korean Applied Science and Technology
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• v.33 no.2
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• pp.286-292
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• 2016

1, 2-Hexanediol galactoside (HD-gal) has been synthesized from 1, 2-hexanediol (HD), a cosmetic preservative, using recombinant Escherichia coli ${\beta}$-galactosidase (${\beta}$-gal) at the high lactose concentration (300 g/l). To confirm the molecular structure of synthesized HD-gal, NMR ($^1H$- and $^{13}C$-) spectroscopy and mass spectrometry of HD-gal were conducted. $^1H$ NMR spectrum of HD-gal showed multiple peaks corresponding to the galactocyl group, which is an evidence of galactocylation on HD. Downfield proton peaks at ${\delta}_H$ 4.44 ppm and multiple peaks from ${\delta}_H$3.96~3.58 ppm were indicative of galactocylation on HD. Up field proton peaks at ${\delta}_H$ 1.60~1.35 ppm and 0.92 ppm showed the presence of $CH_2$ and $CH_3$ protons of HD. $^{13}C$ NMR spectrum revealed the presence of 21 carbons suggestive of ${\alpha}$- and ${\beta}$-anomers of HD-gal. Among 12 carbon peaks from each anomers, the 3 peaks at dC 68.6, 60.9 and 13.2 ppm were assigned to be overlapped showing only 21 peaks out of total 24 peaks. The mass value (protonated HD-gal, m/z = 281.1601) from mass spectrometry analysis of HD-gal, and $^1H$ and $^{13}C$ NMR spectral data were in well agreement with the expecting structure of HD-gal. For further study, the minimum inhibitory concentrations (MICs) of HD-gal against bacteria will be investigated, and, in addition, cytotoxicity to human skin cells of HD-gal will be examined. It is expected that it will eventually be able to develop a new cosmetic preservative, which have low cytotoxicity against human skin cell and maintains antimicrobial effect.