• 제목/요약/키워드: 1D and 2D NMR

검색결과 920건 처리시간 0.024초

A New Steroidal Glycoside from Allium macrostemon Bunge

  • Kim, Yun Sik;Cha, Joon Min;Kim, Dong Hyun;Lee, Tae Hyun;Lee, Kang Ro
    • Natural Product Sciences
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    • 제24권1호
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    • pp.54-58
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    • 2018
  • A phytochemical investigation of Allium macrostemon Bunge (Liliaceae) afforded the new pregnane steroidal glycoside, named allimacroside F (1), along with three known glycosides, benzyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (2), phenylethyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (3), (Z)-3-hexenyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (4). The identification and structural elucidation of a new compound (1) was carried out based on spectral data analyses ($^1H-NMR$, $^{13}C-NMR$, $^1H-^1H$ COSY, HSQC, HMBC, and NOESY) and HR-FAB-MS.

Isolation of Dineolignans, Saucernetin-7 and -8, with Nitric Oxide Inhibitory Activity and NMR assignment from Saururus chinensis

  • Lee, Kyung-Tae;Jung, Hyun-Ju;Park, Hee-Juhn
    • 한국자원식물학회지
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    • 제19권6호
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    • pp.655-659
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    • 2006
  • Two dineolignans (1,2) with nitric oxide inhibitory activities were isolated from Saururus chinensis (Saururaceae) using silica gel column chromatography. Although the structures, saucernetin-7 (1) and -8 (2), have been already reported, NMR assignment of the two compounds was completed aided by 2D-NMR spectroscopy including $^1H-^1H$ COSY, $^1H-^{13}C$ COSY, HMBC and NOESY NMR spectra. Compounds 1 and 2 exhibited significant nitride oxide inhibitory activity in LPS-induced RAW 264.7 cells with $IC_{50}$ values of $11.3{\mu}M\;and\;7.1{\mu}M$, respectively.

순무(Brassica rapa) 뿌리로부터 이차대사산물의 분리 및 동정 (Isolation and identification of secondary metabolites from the roots of Brassica rapa)

  • 방면호;이대영;한민우;정해곤;정태숙;최명숙;이경태;백남인
    • Journal of Plant Biotechnology
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    • 제36권1호
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    • pp.64-67
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    • 2009
  • 순무 뿌리로부터 활성 물질을 분리 동정하기 위하여 80% MeOH 수용액으로 추출하고 이를 여과, 감압 농축하여 MeOH 추출물을 얻었다. 이를 EtOAc 분획, n-BuOH 분획, $H_2O$ 분획으로 나누었으며, EtOAc분획과 n-BuOH 분획에 대해 silica gel 및 ODS column chromatography를 실시하여 4종의 이차대사산물을 분리 정제하였다. $^1H-NMR,\;^{13}C-NMR$, DEPT spectrum 및 mass spectrum등을 통하여 4- (methoxymethyl)phonol(1), ${\alpha}$- methoxy-2, 5- furandimethanel (2), phenyl-${\beta}$-glucopyranoside(3) 및 2-phenylethyl-${\beta}$-D -glucopyranoside (4)로 구조를 결정하였다. 이 화합물들은 순무에서는 처음 분리되었다.

자생 식물로 부터 Cyclin-dependent Kinase 4/Cyclin D1 저해물질의 탐색 (Searching of Cyclin-Dependent Kinase 4/Cyclin D1 Enzyme Inhibition Materials from the Native Plants)

  • 김미란;하지홍;권병목;정하원;안병태;유시용;성낙도
    • Applied Biological Chemistry
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    • 제43권3호
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    • pp.174-178
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    • 2000
  • 인체 세포의 세포주기를 조절하는 Cyclin-dependent Kinase(CDK) 중 CDK4/Cyclin D1 효소 저해 물질을 찾기 위하여 국내에 자생하는 37과 87종의 식물 추출물을 탐색한 결과, 50%$(5\;{\mu}g/ml)$ 이상의 CDK4/Cyclin D1 호소 저해활성을 보인 것은 단삼(Salvia miltiorrhiza), 노박덩굴(Celastrus orbiculatus), 삼백초(Saurus chinensis), 목단(Paeonia suffruticosa) 및 오이풀(Sanguisorba officinalis)이었다. 이들 중에서 목단과 오이풀 추출물이 가장 높은 56%의 저해율을 각각 나타내었다. 또한 추출물에서 활성물질을 추출 정제하여 2차원 NMR 등을 포함한 각종 기기분석을 통하여 cryptotanshinone으로 동정하였다.

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비수리 지상부로부터 분리한 Flavone glycosides (Flavone Glycosides from the Aerial Parts of Lespedeza cuneata G. Don)

  • 권동주;김진규;함연호;배영수
    • Applied Biological Chemistry
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    • 제50권4호
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    • pp.344-347
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    • 2007
  • 비수리 지상부를 95% EtOH 용액으로 추출하고, 추출물을 n-hexane, $CH_2Cl_2$, EtOAc 및 $H_2O$로 용매 분획하였다. 이 중 EtOAc와 $H_2O$ 분획을 대상으로 Sephadex LH-20 column chromatography를 실시하여 4개의 화합물을 분리하였다. 화합물의 구조는 $^{1}H-NMR$, $^{13}C-NMR$, 2D-NMR 및 MS spectrum을 분석하여, quercetin (1), kaempferol (2), desmodin (3) 및 homoadonivernith (4)로 동정하였으며, 그 중 desmodin (3)과 homoadonivernith (4)는 비수리에서 처음으로 분리되었다.

動的 NMR에 依한 $\alpha$-Chlorobenzyl Ethyl Ether의 이온解離速度에 關한 硏究 (A Study on the Ionic Dissociation Rate of $\alpha$-Chlorobenzyl Ethyl Ether by Dynamic NMR Spectroscopy-Chlorobenzyl Ethyl Ether by Dynamic NMR Spectroscopy)

  • 김창렬
    • 대한화학회지
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    • 제24권1호
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    • pp.44-52
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    • 1980
  • 동적 핵자기공명법에 대하여 toluene-$d_8$ 및 carbon tetrachloride 용매속에서의 $\alpha$-chlorobenzyl ethyl ether의 이온해리속도를 측정하였다. 먼저, 동적NMR spectra를 얻고 $J_{AB}, T_2,{\Delta}_{vAB}$ 값 등을 이용하여 computer simulation에 의한 이론spectra를 얻었는데 실측spectra와 매우 잘 일치하였으며, 이로부터 해리속도정수 k를 얻고 이 k의 Eyring plot에 의하여 기울기와 절편의 길이를 알고 이로부터 동력학적 parameter를 얻었다. 이온 해리의 난역도는 용매의 극성에 의존하였으며 활성화 enthalpy는 toluene-$d_8$ 용매중에서 4.7kcal/mole 이었고 carbon tetrachloride 용매중에서 10.7kcal/mole 이었다. 활성화 entropy는 toluene-$d_8$ 용매중에서 -35.8 e.u. 이었고 carbon tetrachloride 용매중에서 -14.4 e.u. 이었다. $S_N$ mechanism의 초기단계로 볼 수 있는 이 이온 해리는 ${\Delta}H^{neq}$ 값이 작아도 비극성 비양자성용매중에서 이온해리가 용역함을 알았으며 작은 ${\Delta}H^{neq}$에 비하여 ${\Delta}S^{neq}$는 음의 큰 값을 가졌음은 주목할 필요가 있다.

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지리터리풀의 플라보놀배당체 (Flavonol Glycoside from the Aerial Part of Filipendula Formosa)

  • 황완균;함인혜;성환길;이무택
    • 약학회지
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    • 제43권1호
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    • pp.5-10
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    • 1999
  • As one of the serial studies on the specific and indigenous plants of Mt. Chiri the constituents of aerial part from filipendula formosa (Rosaceae) were investigated. From of the MeOH extract, five flavonol glycosides, kaempferol-3-O-$\beta$-D-galactopyranoside, querecetin-3-O-$\beta$-D-galactopyranoside, quercetin-3-O-$\alpha$-Lrhamopyranosyl (1 6)-$\beta$-D-galactopyranoside, kaempferol-3-O-$\alpha$-L-rhamnopyranosyl (1 6)-$\beta$-D-galactopyranoside and quercetin-7-O-$\beta$-D-glucopyranosy-3-O-$\beta$-D-galactopyranoside were isolated by column chromatographic separation using Amberlite XAD-2 and Sephadex LH-20, and identified physicochemical evidences (IR, FAB-Mass, $^1H,{\;}^{13}C-NMR$).

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Three Sterol Sulfates Isolated from a Marine Sponge Acanthodoryx Fibrosa

  • Park, Su-Young;Hwang, Byung-Su;Ji, Kwang-Hee;Rho, Jung-Rae
    • 한국자기공명학회논문지
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    • 제11권2호
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    • pp.122-128
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    • 2007
  • Three sterol sulfates were isolated from AMPK activity-guided fraction of a marine sponge Acanthodoryx fibrosa. Their structures were determined by an extensive NMR analysis, MS data, and two compounds were confirmed as unusual phosphorylated sterol sulfates by comparing with NMR data of the known compounds. Compound 3 was given to be a new dephosphated sterol sulfate derivative. Compound 1 moderately showed AMPK activation effect on L6 myoblast cell through Western blot analysis.

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Structure Determination of Four Compounds Isolating from Rhizomes of Rhodiola rosea using NMR Spectrometer

  • Kim, Yun Na;Lee, Jae Sun;Kim, Chul Ho;Jeong, Eun Ju
    • 한국자기공명학회논문지
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    • 제21권4호
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    • pp.145-151
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    • 2017
  • Rhodiola rosea, also known as gold root or rose root, is a perennial plant in the family of Crassulaceae. The rhizhome of R. rosea has been widely used as a hemostatic, tonic for burns and contusions in traditional Chinese medicine. Recent studies reported its strong antioxidant and adaptogenic properties. In this paper, we attempted to isolate compounds from the methanolic extract of R. rosea rhizomes. Four compounds including one new compound (1), two kaempferol glycosides (3 and 4) were isolated from chloroform and ethyl acetate soluble fraction of R. rosea extract. The structures of 1~4 including relative stereochemistry were determined by MS and NMR analysis.

두충엽 함유 퀘르세틴배당체의 함량 표준화 및 계절적 변화 (Standardization and Seasonal Variation of Quercetin Glycoside in Eucommiae Folium)

  • 함인혜;이승재;김호현;강인호;진희억;황완균
    • 생약학회지
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    • 제33권3호통권130호
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    • pp.194-199
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    • 2002
  • The radix and folium of Eucommia ulmoides(Eucommiaceae) has been used for backache, atrophy of the leg and knee, enuresis, hypertension. In order to evaluate to quality of folium, we have been isolated a main compound as a standard compound, which was elucidated $quercetin-3-O-{\beta}-D-xylopyranosyl(l{\rightarrow}2)-{\beta}-D-glucopyranoside$ through it's physicochemical data and IR, FAB-Mass, $^{13}C-NMR$ and $^{1}H-NMR$ analysis. It was analyzed by HPLC system using 17% $CH_3CN$ as a solvent system. The amount of $quercetin-3-O-{\beta}-D-xylopyranosyl(l{\rightarrow}2)-{\beta}-D-glucopyranoside$ from Eucommiae folium was in the range of $0.056{\pm}0.022$ mg(n=7) and also from the results of analysis through seasonal variation$(June{\sim}October)$ September and October have been evaluated to be very high in it's content.