• 제목/요약/키워드: NMR spectroscopic analysis

검색결과 205건 처리시간 0.022초

Streptomyces chromofuscus SMF28을 이용한 Cathepsin B 저해물질의 발효생산 및 특성분석 (Production and Characterization of Cathepsin B Inhibitor from Streptomyces chromofuscus SMF28)

  • 이현숙;김인섭;윤성준;이계준
    • 한국미생물·생명공학회지
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    • 제23권5호
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    • pp.602-608
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    • 1995
  • The aim of the present research program was to construct an optimum fermentation system and to characterize the properties of cathepsin B inhibitor from Streptomyces chromofuscus SMF28. Glucose and casitone were proved to be good carbon source and nitrogen source, respectively. The production of inhibitor was high at lower concentration than 10 mM of inorganic phosphate. The optimum temperature and pH for the production of inhibitor were 30$\circ$C and pH 7, respectively. The production of inhibitor was related to mycelial growth and was affected by medium composition. The inhibitor in culture filtrate of S. chromofuscus SMF28 was purified by butanol extraction, silica gel chromatography, Amberlite IRC-50 (H$^{+}$ form) chromatography, preparative TLC, and preparative HPLC. From amino acid analysis and UV, IR, $^{1}$H-NMR spectroscopic analysis, the inhibitor was identified as a peptide containing valine and phenylalanine derivative.

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Two New Scalaranes from a Korean Marine Sponge Spongia sp.

  • Yang, Inho;Nam, Sang-Jip;Kang, Heonjoong
    • Natural Product Sciences
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    • 제21권4호
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    • pp.289-292
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    • 2015
  • Intensive chemical investigation of Korean marine sponge Spongia sp. has led to the isolation of two new scalaranes. The planar structures of the new compounds 1 and 2 were determined through 1D and 2D NMR spectral data analysis, while the relative stereochemistry of the compounds was determined based on the analysis of $^1H-^1H$ coupling constants and NOESY spectroscopic data. Compounds 1 and 2 did not display any significant biological activities on farnesoid X-activated receptor (FXR) in co-transfection assay.

대두유 에스테르계 절연유의 합성과 분석 (Study on the synthesis and characterization of soybean based transformer oils)

  • 한동희;조한구;한세원;안명상;오대희
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2005년도 하계학술대회 논문집 Vol.6
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    • pp.244-245
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    • 2005
  • Electrical insulation is one of the most important parts in a high voltage apparatus. Traditionally mineral oils and synthetic esters have been widely used as dielectric coolants for power transformers. Recently, researchers are interested in the environmental friendly vegetable oil from environmental viewpoint. This paper reports on the synthesis and characterization of soybean based ester oils. Two different types of soybean based transformer oils, named as methyl ester and isopropyl ester were synthesized. The synthesis of these esters was achieved by transesterification reactions of soybean oil and alcohol in the presence of catalyst. The GC and NMR spectroscopic analysis of the esters have been performed. The thermal stability of the esters was determined by thermal gravimetric analysis(TGA).

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Use of Nuclear Magnetic Resonance Spectroscopy in Analysis of Fennel Essential Oil

  • AbouZid, Sameh
    • Natural Product Sciences
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    • 제22권1호
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    • pp.30-34
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    • 2016
  • A simple and rapid method based on proton nuclear magnetic resonance spectroscopy was developed for determination of trans-anethole content in fennel essential oil. Spectra of pure trans-anethole, of the pure essential oil of fennel, and of the pure oil of fennel with thymol internal standard were recorded. The signal of $H-1^/$ was used for quantification of trans-anethole. This proton signal is well separated in the proton magnetic resonance spectrum of the compound. No reference compound is needed and cheap internal standard was used. The results obtained from spectroscopic analysis were compared with those obtained by gas chromatography. Additionally, the developed method was used for determination of the type of vegetable oil used as a carrier in commercial products, which cannot be quantified as such by gas chromatography. This study demonstrates the application of proton nuclear magnetic resonance spectroscopy as a quality control method for estimation of essential oil components.

천연색소의 과학과 기술 (Science and Technology of Natural Colorants)

  • 정찬희;이정우;류동일
    • 한국염색가공학회지
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    • 제34권2호
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    • pp.77-92
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    • 2022
  • Natural colorants are regarded as substitutes for synthetic colorants in the fields of fiber dyeing, hair dyeing, cosmetic, and food industries. The use of natural colorants has been increased in view of global environment and sustainability. However, scientific approach to the production is required because the supply of natural colorants depends on the climate, soil, and cultivation methods. This brief review contains the advances in science and technology related to natural colorants including characterization, analysis, CIEL*a*b* and Munsell color systems, and future prospects. For the characterization and the analysis of natural colorants, chromatography, some spectroscopic techniques (UV-Vis, FT-IR, NMR), mass spectrometry, and X-ray diffraction are generally used.

Biomass를 위해 제조한 청목노상 callus로부터 Helicobacter pylori 억제물질의 분리 및 동정 (Purification and Identification of Inhibitory Compounds on Helicobacter pylori from Cheongmoknosang Callus for Biomass)

  • 윤동혁;차원섭;이선호;안봉전;김정환;천성숙;배종호;조영제
    • 생명과학회지
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    • 제20권3호
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    • pp.374-380
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    • 2010
  • 청목노상 잎 시료로부터 spot 배양 후 bioreactor에서 배양된 청목노상 뽕잎callus 추출물을 이용하여 H. pylori 균에 대한 항균활성을 측정한 결과, 높은 항균활성을 나타내는 것을 알 수 있었다. 배양된 청목노상 뽕잎 callus 추출물의 H. pylori 균에 대한 항균활성 물질을 정제하여 $^1H$-NMR, $^{13}C$-NMR, IR 및 FAB-MS spectrum 등을 활용하여 구조분석 한 결과 protocatechuic acid, chlorogenic acid, caffeic acid 및 rosemarinic acid로 동정하였으며, 단일물질 보다 혼합물질에 의한 synergy 효과에 의해 H. pylori 균에 대한 항균활성이 나타나는 것으로 판단되었다.

New Cryptand Complexes of Lanthanides(Ⅲ) and Dioxouranium(Ⅵ) Nitrates

  • Oh-Jin Jung;Chil-Nam Choi;Hak-Jin Jung
    • Bulletin of the Korean Chemical Society
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    • 제12권2호
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    • pp.130-137
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    • 1991
  • The following new cryptand 221 complexes of lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate have been synthesized: $(Ln(C_{16}H_{32}N_2O_5)(H_2O)_2(NO_3)_3\ and \((UO_2)_2(C_{16}H_{32}N_2O_5)(H_2O)_4(NO_3)_4$. These complexes have been identified by elemental analysis, moisture titration, conductivity measurements and various spectroscopic techniques. The proton and carbon-13 NMR as well as calorimetric measurements were used to study the interaction of cryptand 221 with La(Ⅲ), Pr(Ⅲ ), Ho(Ⅲ) and $UO_2(Ⅱ)$ ions in nonaqueous solvents. The bands of metal-oxygen atoms, metal-nitrogen atoms and O-U-O in the IR spectra shift upon complexation to lower frequencies, and the vibrational spectra ({\delta}NMN$) of metal-amide complexes in the crystalline state exhibit lattice vibrations below 300 $cm^{-1}$. The NMR spectra of the lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate complexes in nonaqueous solvents are quite different, indicating that the ligand exists in different conformation, and also the $^1H$ and $^{13}C-NMR$ studies indicated that the nitrogen atom of the ring has greater affinity to metal ions than does the oxygen atom, and the planalities of the ring are lost by complexation with metal ions. Calorimetric measurements show that cryptand 221 forms more stable complexes with $La^{3+}$ and $Pr^{3+}$ ions than with $UO^{22+}$ ion, and $La^{3+}/Pr^{3+}$ and $UO^{22+}/Pr^{3+}$ selectivity depends on the solvents. These changes on the stabilities are dependent on the basicity of the ligand and the size of the metal ions. The absorption band (230-260 nm) of the complex which arises from the direct interaction of macrocyclic donor atoms with the metal ion is due to n-{\delta}*$ transition and also that (640-675 nm) of $UO^{22+}$-cryptand 221 complex, which arises from interaction between two-dioxouranium(Ⅵ) ions in being out of cavity of the ligand ring is due to d-d* transition.

Formation of Cadmium(II) Nitrate Complexes with Macrocycles

  • Ho-Doo Kim;Hak-Jin Jung;Oh-Jin Jung
    • Bulletin of the Korean Chemical Society
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    • 제14권5호
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    • pp.561-567
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    • 1993
  • The twelve macrocycle (L) complexes of cadmium(II) nitrate have been synthesized: $CdL(NO_3)_2$. All the complexes have been indentified by elemental analysis, electric conductivity measurements, IR and NMR spectroscopic techniques. The molar electric conductivities of the complexes in water and acetonitrile solvent were in the range of 236.8-296.1 $cm^2{\cdot}mol^{-1}{\cdot}ohm^{-1}$ at 25$^{\circ}$C. The characteristic peaks of macrocycles affected from Cd(II) were shifted to lower frequencies as compared with uncomplexed macrocycles. A complex with 1,4,8,11-tetrakis(methylacetato)-1,4,8,11-tetraaza cyclodecane (L4) exhibited two characteristic bands such as strong stretching (1646 $cm^{-1})$, and weaker symmetric stretching band (1384 $cm^{-1})$. NMR studies indicated that all nitrogen donor atoms of macrocycles have greater affinity to cadmium(II) metal ion than do the oxygen atoms. The $^{13}$C-resonance lines of methylene groups neighboring the donor atom such as N and S were shifted to a direction of high magnetic field and the order of chemical shifts were $L_1 < L_2 < L_3 < L_6 < L_4$. Also the chemical shifts values were larger than those of methylene groups bridgeheaded in side-armed groups. This result seems due to not only the strong interaction of Cd(Ⅱ) with nitrogen donors according to the HSAB theory, but weak interaction of Cd(Ⅱ) and COO- ions or sulfur which is enhanced by the flexible methylene spacing group in side-armed groups. Thus, each additional gem-methyl pairs of L_3, L_4\;and\; L_6$ macrocycles relative to $L_1, L_2,\;and\;L_5$ leads to an large enhancement in Cd(II) affinity. ^{13}C$-NMR spectrum of the complex with $L_{12}$ (1,5,9,13-tetracyclothiacyclohexadecane-3,11-diol) reveals the presence of two sets of three resonance lines, and intensities of the each resonance line have the ratio of 1 : 2 : 2. This molecular conformation is predicted as structure of tetragonal complex to be formed by coordinating two sulfur atoms and the other two sulfur atoms which is affected by OH-groups.

HPLC-ELSD법에 의한 길경의 platycodin D 정량분석 (Quantitative Analysis of Platycodin D from Platycodon grandiflorum by HPLC-ELSD)

  • 김금숙;김현태;성재덕;박희생;김수동
    • 한국약용작물학회지
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    • 제10권3호
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    • pp.200-205
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    • 2002
  • 길경의 부탄올 분획으로부터 지표성분을 분리, 정제하기 위해 $SiO_2$ 컬럼크마토그래피를 실시한 결과 1종(화합물 1)의 단일 물질을 순수 분리하였으며 화합물 1의 구조는 $^1H$, $^{13}C$ NMR 등 분광학적 관측 결과 platycodin D로 확인되었다. Platycodin D의 HPLC 정량법을 검토한 결과, 검출기는 증기화광산란검출기(ELSD)를, 컬럼은 역상컬럼을 사용하여 길경 MeOH 추출액으로부터 효율적인 지표성분 정량이 가능하였다. 추출조건을 재검토한 결과 환류추출보다는 초음파 추출이 더 효율적이었으며 추출용매로는 80% MeOH이 다른 용매조건보다 추출효율이 우수하였다. 건조조건의 검토에서는 platycodin D의 함량이 양건이나 양건과 건조기 혼용건조 보다 건조기 단독 건조시 더 높았으며 특히 $60^{\circ}C$ 열풍건조에서 그함량이 0.083%로서 가장 높았다. 묽은 에탄올 엑스 함량도 건조기만을 이용한 열풍건조가 양건과 건조기 열풍건조를 혼용한 방법보다 4% 정도 더 높았다.

Cytotoxic Compounds from the Stem Bark of Magnolia obovata

  • Min, Byung-Sun;Youn, Ui-Joung;Bae, Ki-Hwan
    • Natural Product Sciences
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    • 제14권2호
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    • pp.90-94
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    • 2008
  • Two sesquiterpenes (1 - 2), a tetralone (3), and two phenylpropanoids (4 - 5) were isolated from the stem bark of Magnolia obovata Thunberg (Magnoliaceae) through repeated column chromatography. Their structures were identified as ${\beta}-eudesmol$ (1), cryptomeridiol (2), 4R-4,8-dihydroxy-${\beta}-tetralone$ (3), trans-pcoumaryl aldehyde (4), and p-coumaric acid (5) on the basis of spectroscopic analysis including two dimensional NMR and mass. Compounds 1 - 3 were tested in vitro for their cytotoxic activity against the K562, HeLa, A549, and HCT116 cancer cell lines. However, compounds 1 - 3 were inactive in this assay system.