• 제목/요약/키워드: NMR and Mass Spectra

검색결과 97건 처리시간 0.02초

Diaminoplatinum(II) Complexes of Glutamic Acid: Obvious Chelating Isomerization

  • Young-A Lee;Jongki Hong;Ok-Sang Jung;Youn Soo Sohn
    • Bulletin of the Korean Chemical Society
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    • 제15권8호
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    • pp.669-673
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    • 1994
  • Coordination isomers of cis-(N-N)Pt(Glu) prepared by reaction of cis-(N-N)Pt($SO_4$) (N-N=2$NH_3$, ethylenediamine(en),(R,R)-1,2-diaminocyclohexane (DACH), N,N,N',N'-tetramethylethylenediamine (TMEDA)) with barium glutamate in water have been monitored and characterized by $^1H-NMR$, $^{13}C-NMR$, IR, and mass spectra. The reaction at room temperature affords the mixture of O,O'-and N, ${\alpha}$ O-chelated platinum(II) complexes. The O,O'-chelate initially formed isomerized to N,${\alpha}$O-chelate on standing for a long time or increasing temperature. The ratio of the two isomers at room temperature depends on the nature of the nitrogen donor coligand (N-N).

Polyacetylene Compounds from Panax Ginseng C. A. Meyer

  • Shim, Sang-Chul;Koh, Hun-Yeoung;Han, Byung-Hoon
    • Bulletin of the Korean Chemical Society
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    • 제4권4호
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    • pp.183-188
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    • 1983
  • Two major and two minor polyacetylenes were isolated from fresh white Korean ginseng roots. The petroleum ether-ethyl ether fractions containing the polyacetylene compounds were collected through solvent fractionation, partition and silica gel column chromatography. Further separation of polyacetylenic fractions was proceeded by bonded normal phase HPLC utilizing a moderately nonpolar microparticulate column. The low pressure liquid chromatography was used for the semi-preparative separation. The chemical structures of the two major polyacetylenes separated were determined by UV, IR, $^1H$ NMR, $^{13}C$ NMR, mass spectra and elemental analysis. One of them is identified to be heptadeca-1-en-4, 6-diyne-3, 9, 10-triol, a new structure, and the other is heptadeca-1, 9-dien-4, 6-diyn-3-ol, known as panaxynol.

New Polyacetylene Compounds from Panax Ginseng C. A. Meyer$^\dag$

  • Shim, Sang-Chul;Chang, Suk-Ku;Hur, Chan-Woo;Kim, Chang-Kew
    • Bulletin of the Korean Chemical Society
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    • 제8권4호
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    • pp.272-275
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    • 1987
  • Two polyacetylene compounds having diyn-ene chromophore were isolated from fresh Korean ginseng roots through solvent fractionation, partition and silica gel column chromatography. The low pressure semi-preparative liquid chromatography and high performance preparative liquid chromatography were used for final separation of polyacetylenic fractions. The chemical structures of these polyacetylenes were determined to be heptadeca-1,8-dien-4,6-diyn-3,10-diol and heptadeca-1,4-dien-6,8-diyn-3,10-diol by UV, FT-IR, $^1H\;NMR,\;^{13}C\;NMR,$ mass spectra and elemental analysis.

방선균 분리주 No. 1882-5로부터 Phorbol Ester에 의해 유도되는 K562 Cell의 소포형성을 억제하는 물질의 분리와 동정 (Purification and Chemical Identification of the Inhibitor on Bleb Formation of K562 Cell Induced by Phorbol Ester from Actinornycetes Isolate No. 1882-5)

  • 안종석;안순철;박문수;김보연;민태익;이현선;오원근
    • 한국미생물·생명공학회지
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    • 제20권5호
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    • pp.565-573
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    • 1992
  • Phorbol ester에 의해 유도되는 K562 cell의 소포 형성을 저해하는 물질을 생산하는 방선균 분리주 No.1882-5를 토양으로부터 분리하였다. 분리주 No. 1882-5로부터 용매추출, Amberlite XAD-4, silica, Lobar low pressure LC를 거쳐 항진균 활성물질 MT-1882-I과 K562 cell의 소포형성을 억제하는 활성물질 MT 1882-II를 분리하였다. 이 물질들에 대한 이화학적 성질의 조사와 UV, $^1H-NMR$, $^13C-NMR$, mass spectrum의 분석에 의하여 MT 1882-II은 piericidin $A_{1}$($C_{25}H_{37}0_4N$, MW 415), MT 1882-II는 glucopiericidin A($C_{31}H_{47}0_9N$, MW 577)로 동정하였다.

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Syntheses and Spectroscopic Studies of Metal-Metal Bonded Complexes (Zr-Fe)

  • Ko, Jae-Jung
    • Bulletin of the Korean Chemical Society
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    • 제7권5호
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    • pp.334-337
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    • 1986
  • The preparation of the metal-metal bonded complex $Cp_2ZrClFeCp(CO)_2$ has been achieved by the reaction of $Cp_2ZrCl_2$ and strong nucleophile $NaFeCp(CO)_2$. The more soluble metal-metal bonded complexes $Cp_2ZrRFeCp(CO)_2(R=CH_3,\;n-C_8H_{17}$) have also been prepared through the reaction of Cp$_{2}$ZrRCl and NaCpFe(CO)$_{2}$. The complexes were characterized by IR, Raman, $^{1}$H NMR and Mass spectra. The complete absorption (100-3800 cm$^{-1}$) spectra for the three metal-metal bonded molecules are reported and the bands of each vibration were assigned.

항암성자원생약개발(抗癌性資源生藥開發)에 관(關)한 연구(硏究) -미국산 개미취근(根)의 성분연구(成分硏究)(II)- (Studies on the Development of Anticarcinomatous Resources -Chemical constituents of the root of Aster divaricatus L. (II)-)

  • 정동규
    • 생약학회지
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    • 제9권2호
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    • pp.73-75
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    • 1978
  • We had previously reported that five compounds were obtained from fraction A of Aster divaricatus by using column chromatography and presumed them to be alkanes $CH_3\;(CH_2)n\;CH_3.$ In this investigation, compound (II) out of above five compounds was identified as hydrocarbon $C_{16}H_{34},$ m.w. 258 belonging to alkane, by using nmr spectra, mass spectra and the elementary analysis. It was also found that compound (IV) is the same compound as the campound (II).

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잔대 추출물과 이들 분획물들의 항산화 및 뇌신경세포 보호 효과 (Antioxidative and Neuroprotective Effects of Extract and Fractions from Adenophora triphylla)

  • 정미자;이상현;박용일;권기한
    • 한국식품영양과학회지
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    • 제45권11호
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    • pp.1580-1588
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    • 2016
  • 잔대의 70% 에탄올 추출물은 강한 항산화 효과 및 산화적 스트레스 조건에서 뇌신경세포 사멸 억제 효과가 있었다. 6개의 분획물 중에 잔대 추출물의 클로로포름 분획물(AT-CH)은 높은 DPPH 라디칼 소거작용 및 세포 내 활성산소종(ROS) 소거작용을 가지고 있었고 $H_2O_2$에 대항하여 뇌신경 세포(SK-N-SH) 보호 효과가 가장 뛰어났다. 활성이 가장 우수한 클로로포름 분획물을 대상으로 주요 물질을 순수분리한 후 $^1H-NMR$, $^{13}C-NMR$ 그리고 EI mass spectra를 이용하여 화학구조를 분석한 결과 phytosterols(${\beta}$-sitosterol과 daucosterol)이라는 것을 알 수 있었다. ${\beta}$-Sitosterol과 daucosterol 역시 산화적 스트레스에 대항하여 SK-N-SH 세포를 보호하는 작용이 있었다. AT-CH 그리고 이것으로부터 분리된 화합물은 p38 경로를 저해하였다. 이들 결과는 AT-CH는 p38 경로를 저해하고 세포 내 ROS 소거작용에 의해 산화적 스트레스로부터 뇌신경세포 보호 효과를 가질 것이라 제안하였다.

Caragana chamlagu Lamarck의 Sterol 성분에 관한 연구 (Studies on the Sterols of Caragana chamlagu Lamarck)

  • 성환길;김일혁
    • 약학회지
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    • 제22권4호
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    • pp.219-225
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    • 1978
  • From the dried roots of Caragana chamlagu Lamarck which have been known to be effective against neuralgia, arthritis, migraine, and sputum, etc. in the folk medicines of Korea, a colorless sterol-like substance, C$_{29}H_{50}O$, m.p. $115-117^{\circ}$, was isolated from the non-saponified fraction of methanolic extract. It was confirmed to be a mixture of four sterols, namely cholesterol, brassicasterol, campesterol, and $\beta$-sitosterol by physico-chemical properties, ir, nmr, mass spectra and gas liquid chromatographic method with the comparison of the authentic samples. In mass fragments of four sterols, furthermore, the same ions of m/e 273, 255, 229 and 213 were assigned to fragments of stigmastane skeletons of the unsaturated phytosterol, and the characteristic ions of each sterol were observed 386, 371, 368, 353 in cholesterol, 398, 383, 380, 365, 355, 337 in brassicasterol, 400, 385, 382, 367 in campesterol and 414, 399, 396, 381 in $\beta$-sitosterol, respectively.

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Mass Fragmentation Patterns as Fingerprints for Positive Identification of Polyphenolic Compounds in a Crude Extract

  • Manshoor, Nurhuda;Weber, Jean-Frederic F.
    • Mass Spectrometry Letters
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    • 제6권4호
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    • pp.105-111
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    • 2015
  • Sixteen compounds of Neobalanocarpus heimii were successfully identified directly from their plant extract using a triple quadrupole LC-MS/MS system. In order to fulfil the objectives of this work, a series of stilbene oligomers of various degrees of condensation were isolated and their structure are characterized. Out of these, four are resveratrol dimers, three trimers, and nine tetramers. The isolation process was done on a fully automated semi-preparative HPLC system. Their structures were elucidated on the basis of 1D- and 2D-NMR as well as MS data. The mass fragmentation patterns of the compounds were recorded and a retrievable in-house library was built to keep the data. In order to demonstrate the potential of this approach, the polyphenolic crude extract was analysed with the LC-MS/MS system and the MS/MS spectra extracted for each chromatographic peak of interest. The fragmentation patterns were compared with those of anticipated pure compounds that were previously recorded. All compounds were successfully identified. It is therefore believed that the LC-MS/MS potential for dereplication of structurally similar compounds in a crude mixture was thus firmly established.

분버들(Salix rorida) 수피의 후라보노이드 및 배당체 화합물 (Flvonoids and Their Glycosides from the Bark of Salix rorida)

  • 함연호;배영수
    • Journal of the Korean Wood Science and Technology
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    • 제30권1호
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    • pp.56-62
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    • 2002
  • 분버들 수피를 아세톤-물(7:3)로 추출한 후 농축하고 헥산, 클로로포름, 에틸아세테이트 및 수용성으로 분획하여 동결건조하였다. 각 추출물은 메탄올 수용액 및 에탄올-헥산 혼합액을 사용하여 Sephadex LH-20 칼럼크로마토그래피로 화합물을 분리한 후 TBA 및 6% 초산에 전개하는 셀룰로오스 박층크로마토그래피로 단리물질을 확인하였다. 단리물질의 화학적 구조는 1H-NMR, 13C-NMR 및 질량 분석으로 결정하였으며, 단일의 화합물로 정제된 물질은 flavonoid와 그 배당체 화합물인 (+)-catechin, naringenin, salipurposide, aromadendrin, isosalipurposide, aromadendrin-7-O-𝛽-D-glucopvranoside 및 taxifolin-7-O-𝛽-D-glucopy- ranoside였다.