• Title/Summary/Keyword: $^{1}H$ NMR

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다슬기로부터 칼슘락테이트의 제조와 품질특성

  • 김순동;이예경;이명예;장경호
    • Proceedings of the Korean Society of Postharvest Science and Technology of Agricultural Products Conference
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    • 2003.04a
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    • pp.122-122
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    • 2003
  • 다슬기의 분말(PSB)과 그 회화분(ASB)으로부터 체내 흡수력이 높은 젖산칼슘의 제조조건과 색상, 용해도 및 관능적 품질을 조사하였다. PSB로부터 제조한 젖산칼슘(PSB-CL)의 PSB 및 젖산 100 mL에 대한 수율은 젖산농도가 10%일 때는 300% 및 15 g, 20%일 때는 260% 및 20 g이었으며, ASB로 제조한 젖산칼슘(ASB-CL)의 ASB 및 젖산 100 mL에 대한 수율은 10% 젖산에서는 400% 및 60 g, 20% 젖산에서는 329% 및 66 g으로 원료량을 기준으로 하였을 때는 다같이 젖산농도의 증가에 따라 감소하였으나 젖산의 부피를 기준으로 하였을 때는 젖산농도의 증가에 따라 증가하였다. Dehydated PSB-CL 및 ASB-CL 제조의 적정온도와 시간은 10$0^{\circ}C$에서는 각각 4 및 5시간, 12$0^{\circ}C$에서는 3 및 4시간, 15$0^{\circ}C$에서는 1 및 2시간으로 ASB-LA의 경우가 짧았다. IR 및 H-NMR spectrum의 분석결과 PBS-LA와 ASB-LA의 구조는 Ca($CH_3$CHOH$CO_2$)$_2$임이 확인되었다. 무수 PSB-CL 및 ASB-CL의 칼슘함량은 각각 15.4%(w/w)와 17.3%(w/w)로 이론 값의 각각 84.2%와 94.5%를 나타내었으며, 미량의 Fe, Na, Mn Zn을 함유하였다. PBS-CL와 ASB-CL의 색상은 각각 연한 황색과 연녹색을 지닌 백색을 띠었다. pH 3~8로 조정한 증류수에서 PSB-CL과 ASB-CL의 평균 용해도는 각각 5.43 g/100 mL 및 6.11 g/100 mL로 standard CL의 4.74 g/mL에 비하여 높았다. 국간장을 제외한 대부분의 액체식품(3% 소금물, 소주, 진간장, 국간장, 포도주스 및 오렌지주스)에서의 용해도는 PSB-CL(3.14~5.03 g/100 mL)과 ASB-CL(4.69~6.05 g/100 mL)이 standard CL(2.94~5.84 g/100 mL)에 비하여 높았다. 관능검사 결과, ASB-CL은 신맛이 낮아 사용범위가 높은 것으로 평가되었으며 PSB-CL는 쓴맛은 높으나 떫은맛이 낮고 구수한 맛이 강하여 식품에의 응용이 기대된다.

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Formaldehyde Free Cross-linking Agents Based on Maleic Anhydride Copolymers

  • Yoon, Kee-Jong;Woo, Jong-Hyung;Seo, Young-Sam
    • Fibers and Polymers
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    • v.4 no.4
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    • pp.182-187
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    • 2003
  • Low molecular weight copolymers of maleic anhydride and vinyl acetate were prepared to develop formaldehyde free cross-linking agents. Since lower molecular weight is favorable for efficient penetration of the finishing agent into the cotton fibers in the padding process, the concentration of the initiator, chain transfer agent and the monomer ratios were varied to obtain copolymers of low molecular weights. The prepared polymers were characterized by GPC, $^1{H-NMR}$, FTIR, DSC and TGA. Copolymers of molecular weights of 2 000 to 10 000 were obtained and it was found that the most efficient method of controlling the molecular weight was by varying the monomer ratios. Poly(maleic anhydride-co-vinyl acetate) did not dissolve in water, but the maleic anhydride residue hydrolyzed within a few minutes to form poly(maleic acid-co-vinyl acetate) and dissolved in water. However, the maleic acid units undergo dehydration to form anhydride groups on heating above ${160}^{\circ}C$ to some extent even in the absence of catalysts. The possibility of using the copolymers as durable press finishing agent for cotton fabric was investigated. Lower molecular weight poly(maleic anhydride-co-vinyl acetate) copolymers were more efficient in introducing crease resistance, which appears to be due to the more efficient penetration of the cross-linking agent into cotton fabrics. The wrinkle recovery angles of cotton fabrics treated with poly(maleic anhydride-co-vinyl acetate) copolymers were slightly lower than those treated with DMDHEU and were higher when higher curing temperatures or higher concentrations of copolymer were used, and when catalyst, $NaH_2$$PO_2$, was added. The strength retention of the poly(maleic anhydride-co-vinyl acetate) treated cotton fabrics was excellent.

Quantitative Analysis of Luteolin 5-glucoside in Ajuga spectabilis and Their Neuroprotective Effects (자란초에서 분리된 Luteolin 5-glucoside의 함량분석과 신경세포 보호 활성)

  • Woo, Kyeong Wan;Sim, Mi Ok;Kim, A Hyun;Kang, Byoung Man;Jung, Ho Kyung;An, Byeongkwan;Cho, Jung Hee;Cho, Hyun Woo
    • Korean Journal of Pharmacognosy
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    • v.47 no.3
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    • pp.211-216
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    • 2016
  • In the course of our continuing search for biologically active components from Korean medicinal plants, we isolated the main compound, luteolin 5-glucoside from aqueous fraction of Ajuga spectabilis. The structure was elucidated by the basis of $^1H$ and $^{13}C$ NMR and TOF ESI-MS data. Quantitative analysis of luteolin 5-glucoside was carried out on a XBridge C18 column ($S-5{\mu}m$, $4.6{\times}250mm$) with gradient elution composed of acetonitrile:water. The results exhibit that the average content of main compound in A. spectabilis were 0.048%. Oxidative stress plays a major role Alzheimer's disease (AD) and other neurodogenerative disease. AD is major health problem and there is currently no clinically accepted treatment to cure or stop its progression. Pretreatment with luteolin 5-glucoside markedly attenuated $H_2O_2$-induced cell viability loss in a dose-dependent manner. Luteolin 5-glucoside also inhibited the formation of intracellular reactive oxygen species in SH-SY5Y. The results suggest that luteolin 5-glucoside from A. spectabilis has protective effects against oxidative stress-induced cytotoxicity, which might be a potential therapeutic compound for treating and/or preventing neurodegenerative disease implicated with oxidative stress.

Preparation of Core-shell Type Nanoparticles of Poly($\varepsilon$-caprolactone) /Poly(ethylene glycol)/Poly( $\varepsilon$-caprolactone) Triblock Copolymers

  • Ryu, Jae Gon;Jeong, Yeong Il;Kim, Yeong Hun;Kim, In Suk;Kim, Do Hun;Kim, Seong Ho
    • Bulletin of the Korean Chemical Society
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    • v.22 no.5
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    • pp.467-475
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    • 2001
  • A triblock copolymer based on $poly(\varepsilon-caprolactone)$ (PCL) as the hydrophobic part and poly(ethylene glycol) (PEG) as the hydrophilic portion was synthesized by a ring-opening mechanism of ${\varepsilon}-caprolactone$ with PEG containing a hydroxyl group at bot h ends as an initiator. The synthesized block copolymers of PCL/PEG/PCL (CEC) were confirmed and characterized using various analysis equipment such as 1H NMR, DSC, FT-IR, and WAXD. Core-shell type nanoparticles of CEC triblock copolymers were prepared using a dialysis technique to estimate their potential as a colloidal drug carrier using a hydrophobic drug. From the results of particle size analysis and transmission electron microscopy, the particle size of CEC core-shell type nanoparticles was determined to be about 20-60 nm with a spherical shape. Since CEC block copolymer nanoparticles have a core-shell type micellar structure and small particle size similar to polymeric micelles, CEC block copolymer can self-associate at certain concentrations and the critical association concentration (CAC) was able to be determined by fluorescence probe techniques. The CAC values of the CEC block copolymers were dependent on the PCL block length. In addition, drug loading contents were dependent on the PCL block length: the larger the PCL block length, the higher the drug loading content. Drug release from CEC core-shell type nanoparticles showed an initial burst release for the first 12 hrs followed by pseudo-zero order release kinetics for 2 or 3 days. CEC-2 block copolymer core-shell type nanoparticles were degraded very slowly, suggesting that the drug release kinetics were governed by a diffusion mechanism rather than a degradation mechanism irrelevant to the CEC block copolymer composition.

Trapping of Methylglyoxal by Sieboldin from Malus baccata L. and Identification of Sieboldin-Methylglyoxal Adducts Forms

  • Kim, Ji Hoon;Zhang, Kaixuan;Lee, Juhee;Gao, En Mei;Lee, Yun Jung;Son, Rak Ho;Syed, Ahmed Shah;Kim, Chul Young
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.245-250
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    • 2021
  • The methylglyoxal (MGO) trapping constituents from Malus baccata L. were investigated using incubation of MGO and crude extract under physiological conditions followed by HPLC analysis. The peak areas of MGO trapping compounds decreased, and their chemical structures were identified by HPLC-ESI/MS. Sieboldin was identified as a major active molecule representing MGO-trapping activity of the crude extract. After reaction of sieboldin and MGO, remaining MGO was calculated by microplate assay method using imine (Schiff base) formation of 2,4-dinitrophenylhydrazine (DNPH) and aldehyde group. After 4 h incubation, sieboldin trapped over 43.8% MGO at a concentration of 0.33 mM and showed MGO scavenging activity with an RC50 value of 0.88 mM for the incubation of 30 min under physiological conditions. It was also confirmed that sieboldin inhibited the production of advanced glycation end products (AGE) produced by bovine serum albumins (BSA)/MGO. Additionally, MGO trapping mechanism of sieboldin was more specifically identified by 1H-, 13C-, 2D NMR and, confirm to be attached to the position of C-3' (or 5').

Thermodynamic and Spectroscopic Analysis of Gas Hydrate-Based $CO_2$ Separation Process (가스 하이드레이트 기반 $CO_2$ 분리 공정의 열역학적 및 분광학적 해석)

  • Park, Sungmin;Lee, Seungmin;Lee, Youngjun;Kim, Yunju;Seo, Yongwon
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.05a
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    • pp.146.1-146.1
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    • 2011
  • 석탄가스화복합발전(IGCC)공정에서 가스화기를 거쳐 생성된 합성가스로부터 $CO_2$를 효과적으로 분리/회수하기 위해 가스 고형화법을 제안하였다. 가스 하이드레이트 형성과정에서의 반응특성을 살펴보기 위하여 반응시간에 따른 가스소모량과 기상의 $CO_2$ 조성 변화를 측정하였다. 순수계와 촉진제 첨가계 (TBAB (10, 40 wt%), TBAF (10, 34 wt%), THF (4, 19 wt%))에 대하여 하이드레이트 생성 후의 기상과 하이드레이트상의 $CO_2$ 조성을 측정하였으며, 그 결과 하이드레이트 형성법에 의해 고농도의 $CO_2$가 하이드레이트상에 포집되는 것을 확인하였다. 가스 소모량 측정실험에서는 THF 19.1 wt%를 첨가하였을 때 가장 큰 소모량을 보였으며, TBAF 10 wt%를 첨가하였을 때 가장 적은 가스소모량을 보였다. $CO_2$ 조성 변화 실험에서는 가스 소모량 실험과 마찬가지로 THF 19.1 wt%를 첨가하였을 때 가장 큰 조성변화를 보였다. 이는 THF의 첨가로 인하여 가스 하이드레이트로의 전환율 증가로 많은 양의 $CO_2$ 기체가 하이드레이트 상에 포집되었음을 나타낸다. 속도론적인 측면에서는 모든 실험조건에서 하이드레이트 형성반응이 1시간 이내에 대부분 종결되는 것을 볼 수 있었다. 또한 $^1H$-NMR을 통하여 혼합가스 하이드레이트의 구조적인 분석을 진행하였다. 본 실험에서 얻어진 결과는 가스 하이드레이트 형성법을 이용한 합성가스 분리 공정 개발에 중요한 기초자료가 될 것으로 사료된다.

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Long-chain alcohols derived from the microalga Monoraphidium

  • Yang, Xuewei;Dai, Xin;Zhang, Rui;Shao, Cong;Geng, Shu;Chen, Guangyi;Liu, Xianhua;Wang, Guangyi
    • Advances in Energy Research
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    • v.1 no.2
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    • pp.107-116
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    • 2013
  • This study was to investigate the composition and characteristics of long-chained alcohols extracted from the algal strain Monoraphidium 3s35. The production of biomass was optimized using different cultivation methods. Under the aerated growth condition, this strain yielded up to 37.26% extracts of dry weight and $576mgL^{-1}$ biomass. The major compounds of the extracts are mainly long-chained alcohols (89.24%), with carbon chain length ranging from 12 to 20. Interestingly, or the long-chained alcohols, 3-(2-Methoxyethyl)-1-nonanol, 3,7,11,15-Tetramethyl-2-hexadecen-1-ol and oleyl alcohol accounted for 53.68%, 23.45%, and 12.11%, respectively. Because of their amphipathic nature, these long-chained alcohols have been widely used in bioenergy production and cosmetics industry. Furthermore, Monoraphidium 3s35 produced 9.73% of $C_{17}$ and $C_{20}$ alkanes, which can be used as an important supplement for the petrodiesel-like fuel.

Antimicrobial Properties and Cytotoxicity of Sulfated (1,3)-β-D-Glucan from the Mycelium of the Mushroom Ganoderma lucidum

  • Wan-Mohtar, Wan Abd Al Qadr Imad;Young, Louise;Abbott, Grainne M.;Clements, Carol;Harvey, Linda M.;McNeil, Brian
    • Journal of Microbiology and Biotechnology
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    • v.26 no.6
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    • pp.999-1010
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    • 2016
  • Ganoderma lucidum BCCM 31549 has a long established role for its therapeutic activities. In this context, much interest has focused on the possible functions of the (1,3)-β-D-glucan (G) produced by these cultures in a stirred-tank bioreactor and extracted from their underutilized mycelium. In the existing study, we report on the systematic production of G, and its sulfated derivative (GS). The aim of this study was to investigate G and its GS from G. lucidum in terms of their antibacterial properties and cytotoxicity spectrum against human prostate cells (PN2TA) and human caucasian histiocytic lymphoma cells (U937). 1H NMR for both G and GS compounds showed β-glycosidic linkages and structural similarities when compared with two standards (laminarin and fucoidan). The existence of characteristic absorptions at 1,170 and 867 cm-1 in the FTIR (Fourier Transform Infrared Spectroscopy) for GS demonstrated the successful sulfation of G. Only GS exhibited antimicrobial activity against a varied range of test bacteria of relevance to foodstuffs and human health. Moreover, both G and GS did not show any cytotoxic effects on PN2TA cells, thus helping demonstrate the safety of these polymers. Moreover, GS showed 40% antiproliferation against cancerous U937 cells at the low concentration (60 μg/ ml) applied in this study compared with G (10%). Together, this demonstrates that sulfation clearly improved the solubility and therapeutic activities of G. The water-soluble GS demonstrates the potential multifunctional effects of these materials in foodstuffs.

Investigation of Siderophore production and Antifungal activity against Phytophthora capsici as related to Iron (III) nutrition by Lysobacter antibioticus HS124

  • Ko, Hyun-Sun;Tindwa, Hamisi;Jin, Rong De;Lee, Yong-Seong;Hong, Seong-Hyun;Hyun, Hae-Nam;Nam, Yi;Kim, Kil-Yong
    • Korean Journal of Soil Science and Fertilizer
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    • v.44 no.4
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    • pp.650-656
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    • 2011
  • Lysobacter antibioticus HS124 isolated from pepper rhizosphere soil produced catechol type siderophore. Purified siderophore by Diaion HP-20 and silica gel column chromatography showed several hydroxyl functional groups adjacent to benzene rings by analysis of $^1H$ NMR spectroscopy. The strain HS124 showed different activities to suppress Phytophthora capsici with different concentrations of exogenous Fe (III) in minimal medium where antifungal activity with $100{\mu}M$ Fe (III) was approximately 1.5 times higher than in absence of Fe (III). Bacterial population in this Fe (III)-amended medium was also highest with $8.9{\times}10^8\;CFU\;ml^{-1}$ which also corresponded to the strongest siderophore activity. When grown in rich medium (minimal medium with N, $P_2O_5K_2O$ and glucose), HS124 exhibited approximately 2 times stronger antifungal activity compared to minimal medium. In pot trials, treatments of bacterial culture grown in rich medium with (C1) or without (C2) $100{\mu}M$ Fe (III) exhibited a high protection of pepper plants from disease, compared to medium only with (M1) or without (M2) $100{\mu}M$ Fe (III). Especially, treatment C1 showed the best disease control effect of about 70 %. Thus, the strain HS124 should be recommended as a potential biocontrol agent against P. capsici in pepper.

Identification of Polyphenol Substances (MP-1) from Seagrass, Phyllospadix Japonica Makino (잘피 게바다말로부터 폴리페놀 물질(MP-1)의 분리 및 동정)

  • Kim, Hae-Seon;Park, Nyun-Ho;Suk, Ho-young;You, Sang-guan;Woo, Jung-Hee
    • Korean Journal of Environmental Agriculture
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    • v.41 no.1
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    • pp.50-54
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    • 2022
  • BACKGROUND: Phyllospadix japonica Makino is a perennial plant belonging to the family Zosteraceae. This species is native to the eastern coast of the Korean Peninsula, and it is found attached to rocks on the seashore. As with all seagrass species, P. japonica is also known to play a major role in protecting the marine environment, and studies on its physiological activities suggestive of its antioxidant, antibacterial and anti-inflammatory potentials have been reported. In this study, purification and structural analysis were performed to identify the polyphenol substances derived from P. japonica. METHODS AND RESULTS: An polyphenol substance MP-1 was purified from the 70% aqueous methanol extract of P. japonica using Diaion® HP-20 column chromatography, ODS column chromatography, and medium-pressure liquid chromatography (MPLC). The purified MP-1 was identified as rosmarinic acid having a molecular weight of 360 and a molecular formula of C18H16O8 through electrospray ionization (ESI)-mass and nuclear magnetic resonance (NMR) spectroscopic analysis. CONCLUSION(S): This study highlights the processes used for the identification of the polyphenol substance derived from P. japonica. Rosmarinic acid, the polyphenol derived from P. japonica identified by this study, is a kind of bioactive substance mainly present in plants. These findings provide an important starting point and are valuable for future studies on bioactive substances in seagrass.