• Journal of the Korean Chemical Society
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• v.50 no.3
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• pp.183-189
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• 2006

A series of substituted styryl 4-methoxy-1-naphthyl ketones [(2E)-1-(4-methoxy-1-naphthyl)-3-phenyl-2-propen-1-ones] were synthesized using facile method of microwave assisted condensation reaction. The yield of chalcones is more than 90%. They are characterized by their physical constants, micro analysis, infrared (KBr, 4000-400 cm？1) and NMR both 1H and 13C spectral data. From infrared spectra, the s-cis and s-trans stretching vibrations of carbonyl group, from NMR spectra the ethylenic proton and carbon chemical shifts (ppm) are assigned. These spectral data are correlated with various Hammett substituent constants. From the results of statistical analysis the effect of substituents on CO, ？ and ？ proton and carbons are explained.

• 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.

• Bulletin of the Korean Chemical Society
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• v.27 no.6
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• pp.893-898
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• 2006

Novel bis- and tris-crown ethers were synthesized from 1-aza and diaza-crown ethers with 2-acryloyloxy-methyl crown ethers through Michael addition. The synthesized bis- and tris-crown ethers were characterized by their elemental analyses, $^1H$-NMR, $^{13}C$-NMR, mass spectra, IR spectra, respectively. The complexation behavior of the bis- and tris-crown ethers with $Li^+$, $Na^+$, $Na^+$, $Rb^+$, $Cs^+$ was examined by $^1H$-NMR, FAB mass, and UV spectrometry.

• Archives of Pharmacal Research
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• v.19 no.4
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• pp.302-306
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• 1996

The $^1H- and^{13}C-NMR$ spectra of alaternin, aurantio-obtusin, chryso-obtusin, obtusin and 2-glucosyl obtusifolin isolated from the seeds of Cassia tora have been assigned based on HMBC, long-range HETCOR, fully $^1H-coupled {13}^C-NMR$, deuterium isotope experiment, and by comparison with the model compounds.

• Korean Journal of Plant Resources
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• v.19 no.6
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• pp.655-659
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• 2006

Two dineolignans (1,2) with nitric oxide inhibitory activities were isolated from Saururus chinensis (Saururaceae) using silica gel column chromatography. Although the structures, saucernetin-7 (1) and -8 (2), have been already reported, NMR assignment of the two compounds was completed aided by 2D-NMR spectroscopy including $^1H-^1H$ COSY, $^1H-^{13}C$ COSY, HMBC and NOESY NMR spectra. Compounds 1 and 2 exhibited significant nitride oxide inhibitory activity in LPS-induced RAW 264.7 cells with $IC_{50}$ values of $11.3{\mu}M\;and\;7.1{\mu}M$, respectively.

• Journal of Microbiology and Biotechnology
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• v.15 no.6
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• pp.1330-1336
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• 2005

Polyhydroxyalkanoic acid (PHA) inclusion bodies were analyzed in situ by $^{13}C$-nuclear magnetic resonance ($^{13}C$-NMR) spectroscopy. The PHA inclusion bodies studied were composed of poly(3-hydroxybutyrate) or poly(3hydroxybutyrate-co-4-hydroxybutyrate), which was accumulated in Hydrogenophaga pseudoflava, and medium-chain-length PHA (MCL-PHA), which was accumulated in Pseudomonas fluorescens BM07 from octanoic acid or 11-phenoxyundecanoic acid (11-POU). The quantification of the $^{13}C$-NMR signals was conducted against a standard compound, sodium 2,2-dimethyl-2-silapentane-5-sulfonate (DSS). The chemical shift values for the in vivo NMR spectral peaks agreed well with those for the corresponding purified PHA polymers. The intracellular degradation of the PHA inclusions by intracellular PHA depolymerase(s) was monitored by in vivo NMR spectroscopy and analyzed in terms of first-order reaction kinetics. The H. pseudoflava cells were washed for the degradation experiment, transferred to a degradation medium without a carbon source, but containing 1.0 g/l ammonium sulfate, and cultivated at $35^{\circ}C$ for 72 h. The in vivo NMR spectra were obtained at $70^{\circ}C$ for the short-chain-length PHA cells whereas the spectra for the aliphatic and aromatic MCL-PHA cells were obtained at $50^{\circ}C\;and\;80^{\circ}C$, respectively. For the H. pseudoflava cells, the in vivo NMR kinetics analysis of the PHA degradation resulted in a first-order degradation rate constant of 0.075/h ($r^{2}$=0.94) for the initial 24 h of degradation, which was close to the 0.050/h determined when using a gas chromatographic analysis of chloroform extracts of sulfuric acid/methanol reaction mixtures of dried whole cells. Accordingly, it is suggested that in vivo $^{13}C$-NMR spectroscopy is an important tool for studying intracellular PHA degradation in terms of kinetics.

• 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.

• Analytical Science and Technology
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• v.17 no.2
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• pp.98-107
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• 2004

In this study, $^1H$ NMR spectroscopy and HPLC were used to identify the type and quantity of each component in an acrylic coating materials applied for an automotive part. By the $^1H$ NMR analysis, it was found that this acrylic coating contained about 88.40 wt% of poly methyl methacrylate (PMMA), 7.05 wt% of methyl methacrylate (MMA), and 2.36 wt% of allyl methacrylate. Polymer additives such as a benzotriazole light stabilizer (Hisorb 328), an oxanilide light stabilizer, butylated hydroxy toluene (BHT), and dimethyl phthalate (DMP) were also identified and measured quantitatively from the $^1H$ NMR spectra. However, only two light stabilizers were identified by reverse phase (RP) HPLC analysis using Bondapak C18 column, methanol mobile phase, and a PDA (Photodiode array) detector. The contents of two light stabilizers in the acrylic coating were measured by a quantitative analysis through UV-Vis spectroscopy and compared with the NMR data. The analytical informations from $^1H$ NMR spetra were better than those from HPLC-PDA plot.

• Bulletin of the Korean Chemical Society
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• v.16 no.12
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• pp.1176-1179
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• 1995

1H NMR spectra of pyridine, α-, β-, and γ-picoline coordinated to the paramagnetic heteropolyanion [Ni3(PW9O34)2]12- (P2Ni3) are reported. NMR lines are assigned to [Ni3(ptl)n(PW9O34)2]12- (n=1, 2 or 3; ptl=pyridine-type ligand) on the basis of their [P2Ni3]/[ptl] dependence. The formation constants for γ-picoline complexes at 25 ℃ are K1=80, K2=610, and K3=190 L mol-1. The monopicoline complex has greater affinity for γ-picoline than P2Ni3. A degradation product, [Ni2(WO2)(PW9O34)2]12-, was also identified at low pH by measuring the NMR spectrum of pyridine coordinated to it. The isotropic NMR shifts come mainly from the contact interaction due to σ-electron delocalization.

• The Korea Journal of Herbology
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• v.23 no.3
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• pp.27-32
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• 2008

Objectives : In this paper, we describe that $^1H-NMR$ spectroscopy may be superior to the conventional HPLC for the quantitative analysis of hesperidin from Citrus unshiu. Methods : $^1H-NMR$ spectra (400 MHz) were recorded in $DMSO-d_6$ using a Varian UNITY Inova AS 400 FT NMR spectrometer. One hundred milligram of powdered Citrus unshiu was weighed out and mixed with 1 ml of $DMSO-d_6$ with sonication for 30 min (room temperature). The extracts were filtrated through a 0.45 ${\mu}m$ PVDF filter and 0.5 ml of filtrated extract used for quantitative $^1H-NMR$ measurement (added 1 mg of dimethyl terephthalate as internal standard). The quantity of hesperidin was calculated by the ratio of the intensity of the compound to the known amount of internal standard. For HPLC analysis, the half gram of plant material was extracted with 60 ml of MeOH for 2 hours. The extracts were made 100 ml volume and analyzed by a Waters HPLC system using a YMC ODS column. The total flow rate was 1.0 ml/min with a sample volume 10 ${\mu}l$ and UV detection at 280nm. Results : The contents of hesperidin in Citrus unshiu was determined $5.33{\pm}0.06$% in the quantitative $^1H-NMR$ method and $5.15{\pm}0.12%$ in HPLC method. Using the quantitative $^1H-NMR$ the contents of hesperidin can be determined in much shorter time than the conventional HPLC measurements. Conclusions : From those results, the advantages of quantitative $^1H-NMR$ analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curve. Besides, it allows rapid and simple quantification for hesperidin with an analysis time for only 10 min without any pre-purification steps.