• Natural Product Sciences
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• 제25권3호
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• pp.222-227
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• 2019

Quantitative nuclear magnetic resonance (qNMR) is a well-established method adopted by international pharmacopoeia for quantitative and purity analyses. Emodin is a type of anthraquinone, well known as the main active component of Fabaceae, Polygonaceae and Rhamnaceae. Purity analysis of emodin is usually performed by using the high-performance liquid chromatography (HPLC)-UV method. However, it cannot detect impurities such as salts, volatile matter, and trace elements. Using the qNMR method, it is possible to determine the compound content as well as the nature of the impurities. Several experimental parameters were optimized for the quantification, such as relaxation delay, spectral width, number of scans, temperature, pulse width, and acquisition time. The method was validated, and the results of the qNMR method were compared with those obtained by the HPLC and mass balance analysis methods. The qNMR method is specific, rapid, simple, and therefore, a valuable and reliable method for the purity analysis of emodin.

• 분석과학
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• 제7권1호
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• pp.91-102
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• 1994

일련의 polypropylene 계통의 공중합체 및 삼중합체 중에서 단량체의 조성에 관한 조성비를 $^{13}C-NMR$ 스펙트럼을 이용하여 정량하였다. 고온에서 얻어진 고분자의 $^{13}C-NMR$ 스펙트럼은 아주 높은 분해능을 보이며, 이는 모든 시그날을 명확하게 지정하는 것을 가능하게 하였으며, 또한 단량체의 조성비를 계산할 수 있도록 하였다. 따라서 단량체의 조성비를 계산하는 방법을 새롭게 제시하였으며, 고분자에서 dyad, triad, tetrad 및 pentad의 조성비도 계산할 수 있다는 것을 보여 주었다. 이러한 단량체 조성에 관한 NMR 분석 결과는 표준 물질을 이용하여 정량한 IR data와 잘 일치한다는 것을 보여 준다.

• Bulletin of the Korean Chemical Society
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• 제19권5호
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• pp.519-524
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• 1998

In this work, we applied the 1D 11B nutation NMR method for the analysis of the local structural environments in powdered borosilicates (SiO2-B2O3). Spin dynamics during a rf irradiation for spin I=3/2 was analytically calculated with a density matrix formalism. Spectral simulation programs were written in MATLAB on a PC. Two borosilicates prepared by the sol-gel process at different stabilization temperature were used for the 1D 11B nutation NMR experiment. The 11B NMR parameters, quadrupole coupling constants (e2qQ/h) and asymmetry parameters (η), for each borosilicate were extracted from the nonlinear least-squares fitting. The effects of heat treatments on the local structures of boron sites in borosilicates were discussed.

• 한국자기공명학회논문지
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• 제16권1호
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• pp.46-66
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• 2012

Metabolomic studies using human urine have shown that human metabolism is altered by a variety of environmental, cultural, and physiological factors. Comprehensive information about normal human metabolite profiles is necessary for accurate clinical diagnosis of disease and for disease prevention and treatment. In this study, metabolite correlation analyses, using $^1H$ nuclear magnetic resonance (NMR) spectroscopy coupled with multivariate statistics, were performed on human urine to compare metabolic differences based on gender and/or obesity in healthy human subjects. First, we applied partial least squares discriminant analysis to the NMR spectral data set to verify the data's ability to discriminate by gender and obesity. Then, the differences in metabolite-metabolite correlation between male and female, and between normal and high body mass index (obese) subjects were investigated through pairwise correlations. Creatine and several metabolites, including isoleucine, trans-aconitate, and trimethylamine N-oxide (TMAO), exhibited different quantitative relationships depending on gender. Dimethylamine had a different correlation with glycine and TMAO, based on gender. The correlation of TMAO with amino acids was considerably lower in obese, compared to normal, subjects. We expect that the results will shed light on the metabolic pathways of healthy humans and will assist in the accurate diagnosis of human disease.

• 대한화학회지
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• 제51권6호
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• pp.520-525
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• 2007

Thiourea/urea, 다양한 aromatic aldehydes, ammonium acetate의 세가지 요소를 가지고 마이크로파의 조 사하에서 무수조건의 활성화된 비산화재를 촉매로 사용하여 높은 수율의 6-aryl-1,2,4,5-tetrazinan-3-thiones/ones를 얻었 다. 6-aryl-1,2,4,5-tetrazinan-3-thiones/ones의 구조는 녹는점, MS, IR, 1H NMR, D2O 교환, 13C NMR, 이차원의 NMR 스펙트럼(HOMOCOR, HSQC)을 바탕으로 증명되었다.

• Journal of Microbiology and Biotechnology
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• 제15권6호
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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.

• Bulletin of the Korean Chemical Society
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• 제28권11호
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• pp.2069-2074
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• 2007

The 27Al multiple quantum magic angle spinning (MQMAS) nuclear magnetic resonance (NMR) spectra of mordenite zeolites were simulated using the point charge model (PCM). The spectra simulated by the PCM considering nearest neighbor atoms only (PCM-n) or including atoms up to the 3rd layer (PCM-m) were not different from those generated by the Hartree-Fock (HF) molecular orbital calculation method. In contrast to the HF and density functional theory methods, the PCM method is simple and convenient to use and does not require sophisticated and expensive computer programs along with specialists to run them. Thus, our results indicate that the spectral simulation of the 27Al MQMAS NMR spectra obtained with the PCM-n is useful, despite its simplicity, especially for porous samples like zeolites with large unit cells and a high volume density of pores. However, it should be pointed out that this conclusion might apply only for the atomic sites with small quadrupole coupling constants.

• 한국양식학회지
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• 제15권3호
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• pp.139-143
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• 2002

해면동물 P. incrustans 시료를 거제도 해금강 연안에서 SCUBA 다이빙에 의하여 채집하였으며, 채집한 시료를 메탄올로 반복해서 추출한 후에 다시 dichloromethane으로 반복 추출하였다 얻어진 유기 조추출물을 n-butanol과 물을 이용하여 분배한 후 n-butanol 층은 다시 15% 메탄올 수용액층과 n-hexane으로 분배하였다. n-Hexane 분배 분획에 대한 silica flash chromatography와 이렇게 얻어진 크로마토그래피 분획에 대한 반복적인 HPLC에 의해서 saringosterol을 분리할 수 있었으며, 이차원적 핵자기 공명 분광기법에 의하여 이 화합물을 구성하는 탄소원자들의 위치를 정확히 지정할 수 있었다. 이 스테로이드는 아직까지 우리나라에서 채집한 해양생물에서는 분리된 적이 없으며 이 화합물의 탄소 위치에 대한 정확한 지정도 처음으로 이루어졌다.

• 한국자기공명학회논문지
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• 제4권2호
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• pp.103-115
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• 2000

Wavelet transforms are introduced as a new tool to distinguish real peaks from the noise contaminated NMR data in this paper. New algorithms of two wavelet transforms including Daubechies wavelet transform as a discrete and orthogonal wavelet transform (DWT) and Morlet wavelet transform as a continuous and nonorthogonal wavelet transform(CWT) were developed fer noise elimination. DWT and CWT method were successfully applied to the noise reduction in spectrum. The inevitable distortion of NMR spectral baseline and the imperfection in noise elimination were observed in DWT method while CWT method gives a better baseline ahape and a well noise suppressed spectrum.

• Bulletin of the Korean Chemical Society
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• 제19권5호
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• pp.501-503
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• 1998

In this work, we applied the 1D $11^B$ nutation NMR method for the analysis of the local structural environments in powdered borosilicates $(SiO_2-B_2O_3)$. Spin dynamics during a rf irradiation for spin I=3/2 was analytically calculated with a density ma trix formalism. Spectral simulation programs were written in MATLAB on a PC. Two borosilicates prepared by the sol-gel process at different stabilization temperature were used for the 1D $11^B$ nutation NMR experiment. The $11^B$ NMR parameters, quadrupole coupling constants $(e^2qQ/h)$ and asymmetry parameters (η), for each borosilicate were extracted from the nonlinear least-squares fitting. The effects of heat treatments on the local structures of boron sites in borosilicates were discussed.