• Title/Summary/Keyword: NMR study

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Antioxidant activity and cell protective effect of loliolide isolated from Sargassum ringgoldianum subsp. coreanum

  • Yang, Xiudong;Kang, Min-Cheol;Lee, Ki-Wan;Kang, Sung-Myung;Lee, Won-Woo;Jeon, You-Jin
    • ALGAE
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    • v.26 no.2
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    • pp.201-208
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    • 2011
  • A monoterpene lactone, loliolide was successively isolated from brown seaweed, Sargassum ringgoldianum subsp. coreanum using column chromatography and high-performance liquid chromatography. The structure of the isolated compound was determined by comparison of EIMS and NMR spectral data with the previously published data. The antioxidant activities of loliolide were also evaluated by DPPH and $H_2O_2$ radical and intracellular reactive oxygen species scavenging assays, and it showed moderate activities in all antioxidant assays. Furthermore, loliolide was found to exert positive dose-dependent effects in the protective effects against $H_2O_2$-induced cell damage which were determined via MTT, Hoechst staining assays and cell cycle analysis. This is the first study on chemical constituent of this seaweed according to our best knowledge. These results clearly indicated that loliolide isolated from Sargassum ringgoldianum subsp. coreanum can protect the cells against $H_2O_2$-induced cell damage or apoptosis.

A Study on reforming product characteristics by gas phase secondary pyrolysis (기상2차 열분해에 의한 개질 생성물 특성에 관한 연구)

  • Son, Young-Il;Yoon, Sang-Jun;Choi, Young-Chan;Ra, Ho-Won;Lee, Jae-Goo
    • 한국신재생에너지학회:학술대회논문집
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    • 2008.05a
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    • pp.243-246
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    • 2008
  • 목질계 바이오매스 가스화 발전에 있어서는 가스화 가스중에 함유되어있는 타르를 가능한 한 가연성 가스로 전환하여 냉가스효율을 향상시키는 것 및 잔유하는 타르는 후단기기에 악영향을 초래할 우려가 있기 때문에 타르를 저감 제거하는 것이 바람직하다. 본 연구에서는 공기 수증기를 사용하여 타르개질 프로세스의 개선을 위해서 타르에서 가스성분으로의 전환에 관한 개질 실험을 실시하여 Wood chip 타르의 열분해 개질 생성물 거동에 대하여 검토하였다. Wood chip 열분해로 생성된 타르의 원소분석 및 $^1H$ NMR분석의 결과로 타르를 치환기를 가지지 않는 방향족, alkyl-기를 가지는 방향족, 산소 함유 방향족, 지방족의 4개로 분류하였다. 개질제에 의해 경질 타르, 중질 타르 모두 감소하였다. 개질 공기는 타르를 연소시키지만 그 속도는 가연성 가스와 경합하고 $900^{\circ}C$에서는 타르의 연소는 나타나지 않았다. alkyl-기를 가지는 방향족은 메탄과 치환기를 가지지 않는 방향족으로 전환되고, 치환기를 가지지 않는 방향족은 수소와 soot로 전환되고, 산소 함유 방향족은 일산화탄소와 치환기를 가지지 않는 방향족으로 전환되는 것을 알았다. 또한, 개질제에 의해alkyl-기를 가지는 방향족, 치환기를 가지지 않는 방향족, 산소 함유방향족 모두가 일산화탄소,이산화탄소로 전환되는 것을 알았다.

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HPLC Analysis and Screening of Standard Compound on Cibotii Rhizoma for Standardization of GCSB-5 Preparation (생약복합제 GCSB-5의 품질 표준화를 위한 구척의 지표성분 탐색 및 HPLC 분석)

  • Cha, Bae-Cheon;Lee, Eun-Hee
    • Korean Journal of Pharmacognosy
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    • v.41 no.1
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    • pp.48-53
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    • 2010
  • GCSB-5 preparation is a purified extract from a mixture of 6 medicinal plants(Acanthopanacis Cortex, Achyranthis Radix, Saposhnikoviae Radix, Cibotii Rhizoma, Glycine Semen Nigra, Eucommiae Cortex) that have been widely used for the treatment of various bone disorders. The aim of this study was to investigate HPLC analysis method and screening of standard compound on Cibotii Rhizoma for quality standardization of a medicinal crude drug GCSB-5. Onitin-4-O-$\beta$-D-glucopyranoside was isolated from Cibotii Rhizoma as the standard compound and identified on the basis of spectroscopic data such as NMR. HPLC analysis method for the determination of onitin-4-O-$\beta$-D-glucopyranoside was established for the quality control of the medicinal plants of Cibotii Rhizoma species, GCSB-5 raw material and GCSB-5 preparation. And validation of HPLC analysis methods were conformed for verification of HPLC methods by check to specificity, linearity, intra-day precision, inter-day precision and accuracy following ICH guideline.

Biopharmaceutical Studies on the Coprecipitate of Metoclopramide-Polyvinylpyrrolidone (Metoclopramide-Polyvinylpyrrolidone 공침물(共沈物)에 관(關)한 생물약제학적(生物藥劑學的) 연구(硏究))

  • Yong, Jae-Ick;Yu, Bong-Shin
    • Journal of Pharmaceutical Investigation
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    • v.10 no.3
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    • pp.33-45
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    • 1980
  • In order to increase the solubility of metoclopramide, various ratio coprecipitates with polyvinylpyrrolidone (M.W. 40,000) were prepared. The experiments of the solubility, physicochemical characteristics were quantitatively developed. The solubility increased as the ratio of rnetoclopramide to polyvinylpyrrolidone in metoclopramide-polyvinylpyrrolindone coprecipitate increased. In powder state, the dissolution rate of metoclopramide-polyvinylpyrrolidone coprecipitate was greater than that of metoclopramide and metoclopramide-polyvinylpyrrolidone physical mixture. Dissolution characteristics of non-disintegrating disk with constant surfacearea was in accord with Noyes-Nernst equation. The intrinsic dissolution rate, G, at $37^{\circ}C$ was $3.98{\times}10^{-7}M/cm^2{\cdot}min$ for metoclopramide, $2.26{\times}10^{-6}\;M/cm^2{\cdot}min$ for 1 : 5 metoclopramide-polyvinylpyrrolidone coprecipitate, respectively. Accordingly, activation energy of metoclopramide was 15,061cal/M, 9,178cal/M for 1 : 5 metoclopramide-polyvinylpyrrolidone coprecipitate and the activation energy decreased as the coprecipitate was formed. X-ray diffraction study revealed the fact that metoclopramide was crystalline, in contrast, there was no crystallinity evident in the 1 : 5 metoclopramide-polyvinylpyrrolidone coprecipitate. There was no difference between physical mixture and coprecipitate in TLC, UV and NMR studies. From the comparision between physical mixture and coprecipitate in IR spectrum, the interaction such as association between metoclopramide and polyvinylpyrrolidone was considered. But the association was easily dissociated in methanol solution.

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High Out-of-Plane Alignment of Liquid Crystalline Methacrylate Copolymer Bearing Photoreactive 4-Styrylpyridine Moiety

  • Kwak, Gi-Seop;Kong, Jong-Yun;Kim, Min-Woo;Hyun, Seok-Hee;Kim, Woo-Sik
    • Macromolecular Research
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    • v.17 no.4
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    • pp.271-275
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    • 2009
  • This paper describes the out-of-plane order of a liquid crystalline(LC) methacrylate copolymer(3) comprised of a methacrylate(1) with a 4-styrylpyridine moiety as the photo-cyclodimerizable group and a benzoate moiety as the mesogenic group in the side chain, and another methacrylate(2) with a 4-(4-methoxyphenyl)benzoate moiety as the mesogenic group. The composition of 1 and 2 units in 3 was estimated to have a molar ratio of 54.2:45.8 by $^{1}H$ NMR spectroscopy. The X-ray diffraction study revealed that the copolymer forms a partial bilayer smectic structure. The copolymer gave rise to a high out-of-plane order parameter of about 0.74 in a wide LC temperature range of $110{\sim}160^{\circ}C$ after linearly polarized, UV light irradiation and subsequent annealing. Moreover, the external reflection IR analysis indicated that excess UV-light irradiation makes the out-of-plane LC structure of the copolymer appear in a higher and wider temperature range.

Structural Characteristics of the Water Soluble Browning Reeaction Products Isolated from Korean Red Ginseng (홍삼으로부터 분리한 수용성 갈변물질의 구조 특성)

  • 이종원;고학룡;심기환
    • The Korean Journal of Food And Nutrition
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    • v.11 no.5
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    • pp.499-505
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    • 1998
  • The purpose of this study was to ivestigate the structural characteristics of waste soulble browning reaction prodcuts (WS-BRPs) isolated from Korean red ginseng. They all showed the maximum absorbances at near 280 nm. Their IR spectra suggested the presence of hydroxyl, amide carbonyl and aliphatic methine groups. From sugar analysis it was identified that L and S-1 contained two kinds of suggar, glucose and xylose, and S-2, a fructose together with glucose and xylose. Thirteen different amino acids were identified in L. Ten amino acids from S-1 and seven amino acids from S-2 were identified using Auto Amino Acid Analyzer. Glycine, serine and glutamic acid in S-1 and one unknown amino acid and glycine in S-2 were detected as the major amino acids, respectively. From the 1H-and 13C-NMR spectra, it was identified that a number of sugar moieties, carbonyl and carbon double bonds (only in S-2) were contained in the three WS-BRP components. Approximate number of sugar moiety of L, S-1 and S-2 was determined to be 8∼10, 9∼11 and 4∼5, respectively. Contents of nitrogen, carbon and hydrogen showed L>S-1>S-2.

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Determination of Polychlorinated Biphenyls in the Soil by Perchlorination (염소화법에 의한 토양 중 Polychlorinated Biphenyls의 잔유분석)

  • Moon, Moon,Chul-Ho;Choi, Choi,Sang-Ki;Kim, Kim,Jung-Ho
    • Journal of Environmental Science International
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    • v.4 no.3
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    • pp.97-97
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    • 1995
  • PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

Determination of Polychlorinated Biphenyls in the Soil by Perchlorination (염소화법에 의한 토양 중 Polychlorinated Biphenyls의 잔유분석)

  • Moon, Moon, Chul-Ho;Choi, Choi, Sang-Ki;Kim, Kim, Jung-Ho
    • Journal of Environmental Science International
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    • v.4 no.3
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    • pp.249-258
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    • 1995
  • PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

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Synthesis of New N2O2 Tetradentate Ligands and Determination of Stability Constants of Metal Complexes for Removal of Heavy Metals (중금속 이온 분리를 위한 새로운 네 자리 N2O2계 리간드의 합성 및 착 화합물의 안정도상수 결정)

  • Kim, Sun-Deuk;Kim, Jun-Kwang;Lee, Kyung-Ho
    • Journal of Environmental Science International
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    • v.16 no.8
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    • pp.913-920
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    • 2007
  • Hydrochloride acid salts of new $N_2O_2$ tetradentate ligands containing amine and phenol N,N'-bis(2-hydroxybenzyl)-o-phenylenediamine(H-BHP), N,N'-bis(5-bromo-2-hydroxybenzyl)-o-phenylenediamine(Br-BHP), N,N'-bis(5-chloro-2-hydroxybenzyl)-o-phenylene-diamine(Cl-BHP), N,N'-bis(5-methyl-2-hydroxybenzyl)-o-phenylene-diamine (Me-BHP) and N,N'-bis(5-methoxy-2-hydroxybenzyl)-o-phenylenediamine(MeO-BHP) were synthesized. The ligands were characterized by elemental analysis, mass and NMR spectroscopy. The elemental analysis showed that the ligands were isolated as dihydrochloride salt. The potentiometry study revealed that the proton dissociation constants$(logK_n{^H})$ of ligands and stability constants $(logK_{ML})$ of transition and heavy metals complexes. The order of the stability constants of each metal ions for ligands was Br-BHP < Cl-BHP > H-BHP < MeO-BHP < Me-BHP.

The Solution Structure of 18 residue YH motif Peptide within the Second fas-1 domain of ${\beta}ig-h3$

  • Han, Kyung-Doo;Son, Woo-Sung;Kim, Won-Je;Lee, Bong-Jin
    • Journal of the Korean Magnetic Resonance Society
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    • v.11 no.1
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    • pp.24-29
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    • 2007
  • [ ${\beta}ig-h3$ ] is an extracellular matrix protein that mediates cell adhesion through interaction with integrins. The 18 residue YH motifs within each fas-1 domain are known to be responsible for the interaction with the ${\alpha}_v{\beta}_5$ integrin, and the synthetic YH motif peptides are known to inhibit endothelial tube formation and reduces the number of blood vessels, and so expected to be an effective inhibitor of angiogenesis. In this study, we solved the 3D structure of the 18 residue YH motif peptide (EALRDLLNNHILKSAMCA; D2 peptide) within the second fas-1 domain of ${\beta}ig-h3$ using NMR. The Peptide has ${\alpha}-helix$ structure at the C terminal region but the N terminal region is flexible. The present structural information may be helpful for developing more effective peptide drug candidate for the treatment of diseases dependent on angiogenesis.

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