• Title/Summary/Keyword: NMR spectrometer

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Quantitative Analysis of t-Cinnamaldehyde of Cinnamomum cassia by $^1H-NMR$ Spectrometry ($^1H-NMR$을 이용한 계피의 t-cinnamaldehyde 정량분석)

  • Song, Myoung-Chong;Yoo, Jong-Su;Baek, Nam-In
    • 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.

A Study on the Chemical Composition and Structure of Sludge, Compost and Charcoal (폐수처리 슬럿지와 퇴비 및 목탄의 화학적 특성과 구조에 관한 연구)

  • 임기표;위승곤
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.35 no.1
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    • pp.27-32
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    • 2003
  • To understand the chemical structure of sewer sludge in comparison with commercial compost and charcoal used as a soil improver, it was carried out to analyse their ash contents and metal ions, and to elucidate the chemical structure of their residuals after a sequential treatment of alcohol-benzene(1:2) extraction in Soxhlet, 3% HCl reflux and 79% H₂SO₄ hydrolysis, using CHNS analyzer and solid C-13 NMR spectrometer. The results obtained were as follows: 1. Ash content of sludge was about 46% that is higher than those of compost (17%) and charcoal (4%). 2. The residual of sludge after a sequential treatment of HCl and H₂SO₄ hydrolyses had high ash content about 23%, too. 3. The sludge seems to be suitable to the soil improver because the content of heavy metal ions in sludge was near the compost and below the organic fertilizer standard. 4. Elemental composition of sludge residual after HCl-H₂SO₄ hydrolyes was C/sub 56/H/sub 91/O/sub 12/N₂S = (C/sub 6/H/sub 10/O/sub 5/)/sub 7/(C/sub 6/H₄)/sub 7/C₂H/sub 43/O₂N₂S, similar to C/sub 103/H/sub 122/O/sub 33/N/sub 6/S = (C/sub 6/H/sub 10/O/sub 5/)/sub 6/(C/sub 6/H₄)/sub 10/C/sub 7/H/sub 22/O₃N/sub 6/S of compost. 5. The sludge residual had proved to have both considerable aliphatic and aromatic groups, but the compost residual to have mainly aliphatic groups and the charcoal to have mainly aromatic groups, through the peak analysis of solid C-13 NMR charts. 6. So, the sewer sludge is proved to have a considerable amount of aromaticity like in woody biomass containing lignin.

Nuclear Magnetic Resonance Study of 23Na in NaMgCl3 Single Crystal (NaMgCl3 단결정 내의 23Na 원자핵에 대한 핵 자기 공명 연구)

  • Yeom, Tae Ho
    • Journal of the Korean Magnetics Society
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    • v.25 no.6
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    • pp.185-188
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    • 2015
  • We have investigated nuclear magnetic resonance of $^{23}Na$ nucleus in $NaMgCl_3$ single crystal in the temperature range 200 K~410 K using FT-NMR spectrometer. The spin-lattice relaxation times $T_1$ of $^{23}Na$ nucleus residing at cubic symmetry in the host crystal was measured as a function of temperature. The $T_1$ of $^{23}Na$ nucleus decreased with increasing temperature. The nuclear spin-lattice relaxation rate $1/T_1$ of $^{23}Na$ in $NaMgCl_3$ single crystal was proportional to the temperature T. This behavior is explained with the characteristic feature of the direct process between the nuclear spins and single phonon, $1/T_1$ being proportional to the absolute temperature. The activation energy calculated was $E_a=4.82J/mol$.

Isolation and Identification of Lipids from the Fruits of Acanthopanax sessiliflorus (오가피(Acanthopanax sessiliflorus Seeman) 열매로부터 지질 화합물의 분리 및 동정)

  • Kim, Su-Yeon;Lee, Dae-Young;Seo, Kyeong-Hwa;Rho, Young-Deok;Kim, Gye-Won;Cheoi, Dae-Sung;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.55 no.2
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    • pp.103-107
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    • 2012
  • Acanthopanax sessiliflorus Seeman fruits (Araliaceae) were extracted at room temperature with 70% aqueous ethanol (EtOH). The concentrated extract was partitioned with ethyl acetate (EtOAc), n-butyl alcohol, and $H_2O$, successively. From the EtOAc fraction, four compounds were isolated through the repeated silica gel and octadecyl silica gel (ODS) column chromatographies. According to the results of physico-chemical and spectroscopic data including NMR, IR, and gas chromatography/mass spectrometer, the chemical structures of the compounds were determined as stigmasterol (1), linoleic acid (2), ${\beta}$-sitosterol (3), and stigmast-5-en-$3{\beta}$,$7{\beta}$-diol (4).

207Pb nuclear magnetic resonance study in PbWO4:Mn2+ and PbWO4:Dy3+ single crystals

  • Yeom, Tae Ho
    • Journal of the Korean Magnetic Resonance Society
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    • v.22 no.4
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    • pp.107-114
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    • 2018
  • In this exploration, the nuclear magnetic resonance of the $^{207}Pb$ nucleus in $PbWO_4:Mn^{2+}$ and $PbWO_4:Dy^{3+}$ Single Crystals using FT-NMR spectrometer is investigated. The line width of the resonance line for the $^{207}Pb$ nucleus decreases as temperature increases due to motional narrowing. The chemical shift of $^{207}Pb$ NMR spectra also increases as temperature decreases for both crystals. The spinlattice relaxation times $T_1$ of $^{39}K$ nucleus were calculated as a function of temperature (180 K~400 K). The $T_1$ of $^{207}Pb$ nucleus decreases as temperature increases. The dominant relaxation mechanism at the studied temperature range can be deduced as the Raman process, which is the coupling between lattice vibrations and the nuclear spins. This deduction is substantiated by the fact that the nuclear spin-lattice relaxation rate $1/T_1$ of the $^{207}Pb$ nucleus in $PbWO_4:Mn^{2+}$ and $PbWO_4:Dy^{3+}$ single crystal is proportional to $T^2$, or temperature squared. The activation energies for the $^{207}Pb$ nucleus in $PbWO_4:Mn^{2+}$ and $PbWO_4:Dy^{3+}$ single crystals are $E_a=49{\pm}1meV$ and $E_a=47{\pm}2meV$, respectively.

녹용의 지질성분 분석과 그 효능에 관한 연구

  • 전길자;조현진;김현정
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1994.04a
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    • pp.175-175
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    • 1994
  • 녹용의 유효성분을 분리하기 위하여 지질성분을 분석하고 그 약효를 검색하였다. Folch-Suzuki 분배법, Sephadex G-50, DEAE-Sephadex A-25 Column Chromatography, High Performance Thin Layer Chromatography, HPLC로 정제한후 Mass Spectrometer, NMR, FT-IR등을 이용하여 구조를 분석하였다. 이 물질은 분자량이 1065인 polyhydroxyunsaturated lipid임을 확인하였다. Strepthzotocin으로 당뇨병을 유발시킨 쥐에 이 물질을 투여한 후 혈액과 조직에서 생화학적 변화를 조사하였다. 정상군에 비해 투여군에서 혈당이 감소하였으나 혈액에서 insulin의 양은 증가하지 않았다. 당뇨병 쥐의 적혈구가 정상에 비해 용혈이 되지 않으나 투여군의 적혈구는 정상과 비숫한 용혈현상을 보여 주었다. 대뇌조직에서 gangliosides를 분석한 결과 당뇨병에 의해 GM1이 증가하는 양상을 보여 주었으나 투여군의 경우 대뇌 gangliosides 분포는 정상과 같았다. 대뇌 lipid bound sialic acid를 정량한 결과 당뇨병에 의해 그 양이 감소되었으나 녹용을 투여하였을 때는 정상에 비해 그 양이 더 증가하였다. Strepthzotocin으로 유발시킨 당뇨병 쥐에 녹용의 지질성분을 투여하였을 때 치료효과가 있는 것으로 추정된다.

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The Synthesis of 9-Phenyl-3,3'-Bis(3-Sulfopropyl)-4,5,4',5'-Naphthothiazolo Carbocyanine Triethyl Ammonium Salt (9-Phenyl-3,3'-Bis(3-Sulfopropyl)-4,5,4',5'-Naphthothiazolo Carbocyanine Triethyl Ammonium Salt의 합성)

  • Kim, Yeoung-Chan
    • Journal of the Korean Applied Science and Technology
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    • v.13 no.3
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    • pp.73-81
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    • 1996
  • In this study, sensitizing dye was prepared by the reaction of 2-methyl-3-sulfopropyl-4,5-naphthothiazolium(inner salt) with triethyl orthobenzoate in the presence of triethylamine. The product was identified by using various analytical tools such as elemental analyzer, IR spectrophotometer, UV-Vis spectrophotometer, $^1H-NMR$ spectrometer, TGA and DSC. Therefore, it was concluded that 9-phenyl-3,3'-bis(3-sulfopropyl)-4,5,4',5'-naphthothiazolo carbocyanine triethyl ammonium salt can be used as red-sensitizing dye for the spectral sensitization of photographic emulsion.

Comparison of Spectral Data of Metabolites Collected from Bruker and Varian 600 MHz Spectrometers

  • Kang, Woo-Young;Chae, Young-Kee
    • Journal of the Korean Magnetic Resonance Society
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    • v.13 no.1
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    • pp.7-14
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    • 2009
  • The spectral data were collected from the two 600 MHz spectrometers from the two major manufacturers, Broker and Varian. The samples were prepared to create standard curves for quantitative measurements of metabolite concentrations. Instead of employing one-dimensional $^1H$ experiments, the two-dimensional $^1H-^{13}C$ HSQC experiments were performed for better separation of resonances. For some resonances, the high salt condition hindered the linear correlation between the intensity and actual metabolite concentration. Excluding overlapped ones, most resonances showed good linearity. Although the Varian spectrometer showed better linearity, both spectrometers were able to generate acceptable standard curves. From this data, we could identify resonances that could be used to better quantify the concentrations of the particular metabolites. With these standard curves, the quantitative measurements of the metabolites from the real samples will be facilitated.

Isolation and Chemical Characterization of Yellow Food Pigments from Monascus Purpureus (Monascus purpureus에서 화색식용색소의 분리 및 화학적 특성)

  • 박영현
    • Journal of Food Hygiene and Safety
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    • v.11 no.2
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    • pp.123-127
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    • 1996
  • The isolation and chemical characterization of yellow food pigments from Monascus purpureus were studied according to the compositions of media. Monacus yellow pigments were isolated and purified by solvent fractionation, silicagel column chromatography, TLC and HPLC. The retention time of Monascus yellow pigments isolated by HPLC was respectively 5 min(I) and 9 min(II) as the yeast malt extract agar(YMA) media and was respectively 4.6 min(III), 5 min(I) 5.7 min(IV), 8.3 min(V), 9 min(II) and 10.7 min(Ⅵ) at the malt extract agar(MEA) media. The structure of monascin(I), ankaflavin(II), 6,11-dihydrorubropunctatin(III), 6,11-dihydromonascorubrin(V) and unknown compounds(IV,Ⅵ) was elucidated by EI-Mass, H and C NMR, UV-visible spectrometer. Therefore, it was suggested that 6,11-dihydrorubropunctatin(III) and 6,11-dihydromonascorubrin(V) are new intermediates of Monascus yellow pigments.

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The Synthesis of Sensitizing Dye for Photographic Emulsion (사진유제용 증감색소의 합성)

  • Kim, Yeoung-Chan;Kang, Tai-Sung;Sohn, Byoung-Chung
    • Journal of the Korean Applied Science and Technology
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    • v.12 no.2
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    • pp.5-11
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    • 1995
  • In the study, sensitizing dye was prepared by the reaction of 2-methyl-3-sulfopropyl-5-phenyl-benzoxazolium(inner salt) with ortho-ester in the presence of triethylamine. The product was identified by using various analytical tools such as Elemental analyzer, IR spectrophotometer, UV-Vis spectrophotometer, $^{1}H$-NMR spectrometer, TGA and DSC. Therefore, it was concluded that benzoxazolo carbocyanine dye can be used as green-sensitizing dye for the spectral sensitization of photographic emulsion.