• Journal of the Korean Magnetic Resonance Society
• /
• v.19 no.1
• /
• pp.18-22
• /
• 2015

The structural geometry of $[N(CH_3)_4]_2CdCl_4$ in a hexagonal phase is studied by $^1H$ MAS NMR, $^{13}C$ CP/MAS NMR, and $^{14}N$ NMR. The changes in the chemical shifts for $^{13}C$ and $^{14}N$ in the hexagonal phase are explained by the structural geometry. In addition, the temperature dependencies of the spin-lattice relaxation time in the rotating frame $T_{1{\rho}}$ for $^1H$ MAS NMR and $^{13}C$ CP/MAS NMR are measured.

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

• Microbiology and Biotechnology Letters
• /
• v.33 no.2
• /
• pp.123-129
• /
• 2005

Isolation and identification of pathogens from slaughter and meat processing plant were investigated. Antimicrobial activity of Amaranthus lividus against isolated pathogens such as Aeromonas sobria, Escherichia coli, Escherichia coli O157, Listeria monocytogenes, Salmonella spp., and Staphylococcus aureus was investigated. Among the chloroform, ethyl acetate and buthanol fraction of amaranthus lividus showed inhibitory effect against Aeromonas sobria CLFM1 and Escherichia coli CLFM2. Antimicrobial substance in chloroform fraction was isolated by silica gel adsorption column chromatography, sephadex LH-20 column chromatography and silica gel partition column chromatography. The antimicrobial compound of amaranthus lividus was identified as diethyl phtalate by HPLC, GC-MS, H-NMR and C-NMR.

• Bulletin of the Korean Chemical Society
• /
• v.14 no.6
• /
• pp.722-726
• /
• 1993

Organotin(IV) complexes of ylidenemalonates $(R_xSn)_{x-1}(O_2C)_2C=C(SR')_2\;(R=n-C_4H_9,\;C_6H_5,\;cyclo-C_6H_{11},\;CH_3OOCCH_2CH_2;\;x=2,3;\;R'=CH_3,\;R_2'=-CHCH-,\;-CH_2CH_{2^-})$ have been synthesized and characterized by means of various spectroscopic methods. The X-ray crystal structure of $(Ph_3Sn)_2(O_2C)_2C=C(SCH_3)_2$ has been determined (Pi; a= 9.704(2) ${\AA}$, b= 14.412(1) ${\AA}$, c= 14.760(3) ${\AA}$, ${alpha}$=74.26(1)$^{\circ}$, ${beta}$=99.38(l)$^{\circ}$, ${\gamma}$=79.09(1)$^{\circ}$, $V= 1950.7(7){\AA}^3$) and refined to R= 0.045. The crystal structure discloses a discrete molecule with bidentate-like carboxylate ligand. For diorganotin analogues, the structures are discussed in terms of IR, $^1H-NMR,\;^{13}C-NMR$, and FAB mass spectrometry. The mass spectrum indicates that the diorganotin complexes of ylidenemalonates are dimeric.

• Analytical Science and Technology
• /
• v.14 no.1
• /
• pp.1-7
• /
• 2001

6,6-Dichlorobicyclo[3, 1, 0]hexane-3carboxylic acid was synthesized by dichlorocarbene addition into 3-cyclopentenecarboxylic acid using BTEA.Cl as phase transfer catalyst. $^1H$ NMR $^{13}C$ NMR data analyst showed that this compound had boat-like conformation and carboxyl group existed as trans form.

• Journal of the Korean Chemical Society
• /
• v.37 no.1
• /
• pp.43-48
• /
• 1993

The $^1H-NMR$ spectra of the NH-group were obtained for N-ethylacetamide (NEAA) in the series of n-alcohols over a temperature range of 310∼350K by using NMR spectroscopy. The $^1H-NMR$ lineshape coupled to $^{14}N$ nucleus were analyzed to obtain the reorientational correlation times ${\tau}_c$ of NEAA. The data indicate that the coupling of solute and solvent decreases as the chain length of n-alcohols increases. But in the n-alcohols the reorientational motion depends almost linearly on η/T of solvents over our temperature range. The results are discussed in the context of the subslip phenomenon.

• Applied Biological Chemistry
• /
• v.46 no.2
• /
• pp.69-73
• /
• 2003

A novel antifungal antibiotic for azole-resistant Candida albicans was purified from the culture broth of Bacillus subtilis LAM 97-44 by butanol extraction, Diaion HP-20 and Dowex-50 adsorption chromatography, silica gel flash chromatography followed by HPLC and designated LAM-44A. LAM-44A was stable for 60 min at $100^{\circ}C$, and pH range from 2 to 10. MIC values were observed at $0.5-3.5\;{\mu}g/ml$ against various Candida albicans strains. The antibiotic showed no cytotoxicity for S180, MKN-45, P388, HeLa and 373 at the concentration of 1 mg/ml. LAM-f4A was colorless powder soluble in water, methanol, ethanol, butanol and negative to ninhydrin reaction. The antibiotic had maximum absorption at 273 nm in methanol, and melting point was $202^{\circ}C$. The molecular weight and formula were determined to be 282 and $C_{14}H_{34}O_5$ by $^1H-NMR,\;^{13}C-NMR$, IR spectrum and elemental analysis.

• Journal of the Korean Applied Science and Technology
• /
• v.38 no.3
• /
• pp.824-831
• /
• 2021

1, 2-Octanediol galactoside (OD-gal) has been synthesized from 1, 2-octanediol (OD), as a safer cosmetic preservative, using recombinant Escherichia coli β-galactosidase (β-gal). To confirm the molecular structure of synthesized OD-gal, mass spectrometry and NMR (¹H- and ¹³C-) spectroscopy of OD-gal were carried out. In the reaction mixture, a sodium adduct ion of OD-gal (m/z=331.1732) was identified using mass spectrometry analysis. In addition, ¹H NMR spectrum of OD-gal showed multiple peaks corresponding to the galactosyl group, which is evidence of galactosylation on OD. Downfield proton peaks at δ_H 4.39 ppm and multiple peaks from δ_H 3.98~3.55 ppm were indicative of galactosylation on OD. Up field proton peaks at δ_H 1.52~1.26 ppm and 0.89 ppm showed the presence of CH₂ and CH₃ protons of OD. ¹³C NMR spectrum revealed the presence of 24 carbons suggestive of α- and β-anomers of OD-gal. Among 14 carbon peaks from each anomer, the 4 peaks at δ_C 31.4, 29.0, 22.3, and 13.7 ppm were assigned to be overlapped showing only 24 peaks out of a total of 28 peaks. The mass value from mass spectrometry analysis of OD-gal, and ¹H and ¹³C NMR spectral data were in good agreement with the expecting structure of OD-gal. Finally, we identified a galactose molecule from the hydrolysate of OD-gal using β-gal. We are expecting that through future study it will eventually be able to develop a safe cosmetic preservative.

• Natural Product Sciences
• /
• v.4 no.3
• /
• pp.153-157
• /
• 1998

The aqueous ethanolic leaf extract of Ailanthus altissima was found to contain the new natural product, $luteolin\;7-O-{\beta}-(6"-galloylglucopyranoside)$, 13, along with fourteen known phenolic metabolites (1-12, 14 and 15). Structures of all compounds (1-15) were established by conventional methods of analysis and confirmed by FAB-MS, $^1H-\;and\;^{13}C-NMR$ spectral analysis.

• Journal of the Korean Applied Science and Technology
• /
• v.36 no.1
• /
• pp.84-89
• /
• 2019

To characterize the molecular structure of BzO-gal synthesized using Escherichia coli ${\beta}$-gal, NMR ($^1H$- and $^{13}C$-) spectroscopy and mass spectrometry of BzO-gal were conducted. $^1H$ NMR spectrum of BzO-gal showed multiple peaks corresponding to the galactosyl group, which is an evidence of galactosylation on BzOH. Five proton peaks around the aromatic region at ${\delta}_H$ 7.43 ~ 7.24 ppm and 2 peaks from ${\delta}_H$ 4.93 and 4.67 ppm were evidence of the presence of the benzyl group. Seven proton peaks at ${\delta}_H$ 4.32 ~ 3.46 ppm showed the presence of a monosaccharide and were indicative of galactosylation on BzOH. $^{13}C$ NMR spectrum also revealed the presence of 11 carbons suggestive of BzO-gal. The mass value (sodium adduct ion of BzO-gal, m/z = 293.0994) from mass spectrometry analysis of BzO-gal, and $^1H$ and $^{13}C$ NMR spectral data were in good agreement with the expecting structure of BzO-gal. We are expecting that through future study it will eventually be able to develop a new additive of low cytotoxicity.