• 제목/요약/키워드: $^1H$ and $^{13}C$ NMR

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Pseudomonas sp. RRj 228이 분비하는 항균물질의 동정과 고추탄저균 C. acutatum에 대한 항균활성 (Structural Identification of Antibiotics from Pseudomonas sp. RRj 228, a Antifungal Activity of Collectotrichum acutatum Causing Anthracnose on Pepper)

  • 전상윤;김용균;손홍주;박현철;이상몽;김선태;박기도;강위금;김근기
    • 생명과학회지
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    • 제20권8호
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    • pp.1254-1260
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    • 2010
  • 식물 근권미생물은 식물의 뿌리 표면과 내부에 정착하면서 식물생장 촉진물질을 분비하여 식물생육에 직접적인 영향을 주거나, 항균물질을 분비하여 병원균으로부터 식물 근권환경을 보호하여 식물의 생육을 촉진하게 된다. 이러한 활성을 갖고 있는 미생물을 분리하여 동정하며, 항균물질을 분리, 동정하여 지속농업의 발전과 농업환경의 보전을 위하여 연구를 실시하였다. 논토양으로부터 식물생육촉진활성과 항균활성을 갖는 RRj 228균주를 분리하여, 생리 생화학적방법과 유전학적 방법으로 동정한 결과, Pseudomonas sp.로 동정되었다. RRj 228균주는 B. cinerea, P. ultimum, P. capsici와 R. solani에도 높은 항균활성을 보였으며, 특히 고추탄저병원균인 C. acutatum에 강력한 항균활성을 나타냈다. RRj 228균의 배양여액을 C. acutatum, R. solani 및 P. ultimum에 대한 $ED_{50}$값을 측정한 결과 0.14, 0.16, 0.29 mg/ml로 나타났다. 항균활성물질은 RRj 228 배양여액으로부터 각종 크로마토그라피법으로 순수분리하고, NMR과 GC/MS 등의 기기분석을 실시하여 구조를 Phenazine-1-carboxylic acid (분자량 224)로 동정하였다.

SQUID 센서 기반의 극저자장 자기공명 장치를 위한 사전자화코일 전류구동장치 개발 (Development of Prepolarization Coil Current Driver in SQUID Sensor-based Ultra Low-field Magnetic Resonance Apparatuses)

  • 황성민;김기웅;강찬석;이성주;이용호
    • Progress in Superconductivity
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    • 제13권2호
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    • pp.105-110
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    • 2011
  • SQUID sensor-based ultra low-field magnetic resonance apparatus with ${\mu}T$-level measurement field requires a strong prepolarization magnetic field ($B_p$) to magnetize its sample and obtain magnetic resonance signal with a high signal-to-noise ratio. This $B_p$ needs to be ramped down very quickly so that it does not interfere with signal acquisition which must take place before the sample magnetization relaxes off. A MOSFET switch-based $B_p$ coil driver has current ramp-down time ($t_{rd}$) that increases with $B_p$ current, which makes it unsuitable for driving high-field $B_p$ coil made of superconducting material. An energy cycling-type current driver has been developed for such a coil. This driver contains a storage capacitor inside a switch in IGBT-diode bridge configuration, which can manipulate how the capacitor is connected between the $B_p$ coil and its current source. The implemented circuit with 1.2 kV-tolerant devices was capable of driving 32 A current into a thick copper-wire solenoid $B_p$ coil with a 182 mm inner diameter, 0.23 H inductance, and 5.4 mT/A magnetic field-to-current ratio. The measured trd was 7.6 ms with a 160 ${\mu}F$ storage capacitor. trd was dependent only on the inductance of the coil and the capacitance of the driver capacitor. This driver is scalable to significantly higher current of superconducting $B_p$ coils without the $t_{rd}$ becoming unacceptably long with higher $B_p$ current.

Development of Gradient Centrifugal Partition Chromatography Method and Its Application for the Isolation of 3,5-Dimethoxyphenanthrene-2,7-diol and Batatasin-I from Dioscorea opposita

  • Yoon, Kee-Dong;Yang, Min-Hye;Chin, Young-Won;Kim, Yoen-Jun;Kim, Hye-Ryung;Choi, Ki-Ri;Park, Ju-Hyun;Kim, Jin-Woong
    • Natural Product Sciences
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    • 제15권3호
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    • pp.144-150
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    • 2009
  • Gradient centrifugal partition chromatography (GCPC) method was developed and applied to isolate 3,5-dimethoxyphenanthrene-2,7-diol (DMP) and batatasin-I (BA-I) from the dichloromethane soluble extract of Dioscorea opposita. In this method, the lower phase of n-hexane-methanol-water system (HMW, 10 : 9 : 1, v/v) was used as a mobile phase A (MpA) and water was used as a mobile phase B (MpB). This gradient CPC method is comparable to that of reversed-phase HPLC method in that the stationary upper-phase of HMW (10 : 9 : 1 v/v) works as if it were reversed-phase silica gel due to its hydrophobic property, while the lower phase (MpA) and water (MpB) functioned as hydrophilic mobile phases. The initial condition of the mobile phase was 20% MpA/80% MpB and maintained for 150 min to obtain DMP (1.2 mg), and then MpA was increased up to 50% to elute BA-I (1.7 mg). The purities of DMP and BA-I were 94.1% and 98.3% with the recovery yields of 83% and 86%, respectively. Similar results were obtained by linear-gradient CPC. The CPC peak fractions were identified by comparing their retention time to those of authentic samples of DMP and BA-I and their spectroscopic data ($^1$H NMR and $^{13}$C NMR) to those of literature values.

Studies on Biological Activity of Wood Extractives (XVII) - Components and Antioxidant activity of Alnus firma -

  • Choi, In-Ho;Choi, Tae-Ho;Park, Youngki;Lee, Oh-Kyu;Kwon, Yeong-Han;Kang, Ha-Young;Park, Il-Kwon;Choi, Don-Ha;Shin, Sang-Chul;Lee, Hak-Ju
    • Journal of the Korean Wood Science and Technology
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    • 제34권2호
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    • pp.95-100
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    • 2006
  • This study is to isolate bio-active compounds from Alnus firma and evaluate their antioxidant activity. Dried wood powder of A. firma was extracted by organic solvents and fractionated in the sequential extraction steps. The isolated compounds were characterized by EI-MS, $^{13}C-$ and $^1H-NMR$ including COSY, DEFT, HMQC, and HMBC. Antioxidant activities of the isolated compounds were evaluated by DPPH (1,1-diphenyl-2-picrylhydrazyl) free radical scavenging effect. From the wood of A. firma, three kinds of diarylheptanoids, alnusodiol (1), alnusonol (2) and alnusone (3), and gallic acid (4) were isolated. Among these four compounds, compound 1, 2, and 3 are isolated from A. firma for the first time. The antioxidant activity of gallic acid was 93.5% at the concentration of 100 ppm. This compound showed stronger antioxidant activity than those of other isolated compounds and the reference BHT (butylated hydroxytoluene).

Synthesis of Novel Polythiol for Plastic Optical Lens and its Ophthalmic Lens

  • Jang, Dong-Gyu;Roh, Soo-Gyun;Kim, Jong-Hyo;Jin, Wen-Yi;Seo, Jin-Moo;Kwon, Myeong-Ja;Lee, Soo-Min
    • Bulletin of the Korean Chemical Society
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    • 제30권10호
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    • pp.2227-2232
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    • 2009
  • Novel polythiol materials of urethane lens series for plastic optical lens were synthesized from polyol materials via thioisouronium of thiourea with c-HCl in refluxing aqueous solution, in which polythiol material was carried out from hydrolysis of thioisouronium by ammonia water. Their structure properties were identified by EA, EI-MS, FT-IR, $^1H\;and\;^{13}C$ NMR spectroscopies and TGA. Their ophthalmic lenses as polythiourethane material were prepared by thermal curing to an injected glass mold using the evenly solutions of diisocyanates series (TDI, XDI, HDI or IPDI) with polythiols. Polythiourethane shows that the strong stretching mode for SH group of polythiol disappeared in FT-IR spectra after thermosetting polymerization. Thermal deformation starting temperature of ophthalmic lenses was determined by TMA. Ophthalmic lenses made from characteristic polythiol and diisocyanate series have transparency, colorless and good impact strength, in which thermal resistance and impact strength of ophthalmic lenses were influenced by diisocyanate series. Physical properties of ophthalmic lens have contrast thermal resistance with impact strength. The property of thermal resistance and impact strength for respective ophthalmic lenses was examined by TMA and drop ball test.

고비로부터 Cinnamtannin B-1의 분리 및 함량 분석 (Isolation and Quantitative Analysis of Cinnamtannin B-1 from Osmunda japonica Thunb)

  • 김민석;우경완;이기호;이현주;이선유;강병만;전병훈;조정희;조현우
    • 생약학회지
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    • 제47권3호
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    • pp.232-236
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    • 2016
  • In traditional Korean medicine, Osmunda japonica Thunb has been used as hemostasis and antipyretic treatment. The main compound "cinnamtannin B-1" was obtained by column chromatographic separation, and its structure was determined by spectroscopic methods, including $^1H$, $^{13}C$ NMR, and IT-TOF-ESI MS. Ash, moisture and extract content and acidinsoluble ash were monitored as identification test to establish the analytical methods. The optimum reflux extraction condition was 100% methanol extracted 30 min for 2 times. A quantitative analysis using HPLC method exhibited that the main compound at 24.7 min and its content was 0.96% in methanol extraction.

섬바디로부터 L. monocytogenes에 대한 생장억제 물질의 분리 및 구조동정 (Isolation and Identification of Growth Inhibition Substance on L. monocytogenes from Dystaenia takesimana Kitagawa)

  • 오진아;신동화;백남인
    • 한국식품과학회지
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    • 제31권4호
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    • pp.984-993
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    • 1999
  • 섬바디 75% 에탄올 추출물과 핵산 분획물을 첨가하여 Listeria monocytogenes(Lm) ATCC 19111, ATCC 19112, ATCC 19113, ATCC 19114 및 ATCC 15313에 대한 증식억제 효과와 그 활성 물질의 구조를 확인하였다. 항균효과를 시험한 결과 에탄올 추출물은 50 ppm, 핵산 분획물의 경우에는 30 ppm에서 5종의 Listeria 균주를 모두 증식저해 시켰다. 항균활성이 우수한 섬바디 핵산 분획물을 silica gel column으로 1회 분획하여 획분 A8을 얻었고 이의 항균효과는 대단히 우수하여 10 ppm에서 실험균주 모두를 증식저해 시켰다. A8이 아주 우수한 항균효과를 나타내었기에 살균효과가 기대되었다. Tryptic soy broth에 섬바디 추출물에서 분리된 A8를 30 및 10 ppm씩 배지에 첨가한 후 Lm 5균주를 배양시켜 24시간 간격으로 생균수를 확인한 결과 대조구는 균수가 증가하는 반면 처리구는 균수가 감소함으로서 살균효과가 인정되었다. 그리고 이 획분 A8을 2회 연속 분리하여 단리된 소획분 SBD-1과 SBD-2를 얻었다. 이렇게 단일 물질로 분리된 SBD-1과 SBD-2의 항균효과는 column 분리후 얻은 획분(A8)보다 증식억제 효과가 감소하였는데 이는 섬바디에 존재하는 항균물질은 단독으로 작용하는 것이 아니라 그 안에 있는 여러 물질들의 혼합작용으로 그 효과가 나타난 것이라 추정되었다. 단일물질로 분리된 두 물질 중 수율이 높은 SBD-2를 구조 동정한 결과 폴리아세틸렌 화합물 (9z)-hepta-deca-1,9-dien-4,6-diyn-3,8-diol 인 falcarindiol로 확인되었다. 이 물질은 미나리과 식물 뿌리에 존재한다.

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Inhibitors of Tyrosinase and Melanogenesis from Galla rhois

  • Kim, Hyo-Jin;Jang, Dong-Il;Park, Sang-Won
    • Preventive Nutrition and Food Science
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    • 제2권4호
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    • pp.285-290
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    • 1997
  • Previously, a 50% aqueous methanol extract of Galla rhois was shown to be the most potent tyrosinase inhibition activity with an {TEX}$IC_{50}${/TEX}(the concentration causing 50% inhibition of tyrosinase activity) of 0.2mg/ml of 205 crude drug extracts. To isolate tyrosinase inhibitors, the methanol extract was evaporated to a small volume in vacuo, and then partitioned stepwise with benzene and ethyl acetate(EtOAc). the EtOAc fraction was solubilized in 10% MeOH solution, and then fractionated successively by Diaion HP-20 and Sephadex LH-20 column chromatography, and preparative HPLC. Three phenolic compounds were isolated, and characterized as gallic acid(GA), methyl gallate(MG) and 1,2,3,4,6-penta-O-galloyl-$\beta$-D-glucose(PGG) by UV, IR, {TEX}${1}^H${/TEX}-&{TEX}${13}^C${/TEX}-NMR, and FAB-MS spectroscopy, PGG({TEX}$IC_{50}${/TEX}=50$\mu\textrm{g}$/ml) showed a considerable inhibitory effect against mushroom tyrosinase, while GA({TEX}$IC_{50}${/TEX}=1.6mg/ml) and MG({TEX}$IC_{50}${/TEX}=234$\mu\textrm{g}$/ml) did not show an appreciable effect. Meanwhile, MG inhibited greatly melanogenesis in a murine melanocyte cell line, Mel-Ab. MG and PGG showed typical noncompetitive inhibition patterns against mushroom tyrosinase. These results suggest that PGG and MG may be potentially useful as either anti-browning or anti-melanogenic agents in foods and cosmetics.

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Syntheses and Evaluations of Antitumor and Antiangiogenic Phthalate Polymers Containing 5-Fluorouracil and Carboxylates

  • Lee, Sun-Mi;Jung, Sang-Wook;Ha, Chang-Sik;Chung, Il-Doo;Lee, Won-Ki;Park, Yong-Ho
    • Macromolecular Research
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    • 제16권6호
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    • pp.510-516
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    • 2008
  • New antitumor active polymers, poly(methacryloyl-2-oxy-1,2,3-propanetricarboxylic acid-co-exo-3,6-epoxy-l,2,3,6-tetrahydrophthalic acid) [poly(MTCA-co-ETAc)], poly(methacryloyl-2-oxy-l,2,3-propanetricarboxylic acid-co-hydrogen ethyl-exo-3,6-epoxy-l,2,3,6-tetrahydrophthalate) [poly(MTCA-co-HEET)], and poly(methacryloyl-2-oxy-l,2,3-propanetricarboxylic acid-co-a-ethoxy-exo-3,6-epoxy-1,2,3,6-tetrahydrophthaloyl-5-fluorouracil) [poly(MTCA-co-EETFU)] were synthesized and characterized. Their antitumor activity, inhibition of DNA replication and antiangiogenesis were examined. The structures of the polymers were identified by FT-IR, $^1H$ and $^{13}C$-NMR spectroscopy. The number average molecular weights of the fractionated polymers determined by GPC ranged from 9,400 to 14,900, and polydispersity indices were less than 1.7. The in vitro cytotoxicity of these polymers was determined and their antitumor activity was evaluated. The $IC_{50}$ values (the drug concentration at inhibition of 50% tumor growth) indicated that the synthesized polymers were much better inhibitors of cancer cells and showed lower cytotoxicity than the free 5-FU. The in vivo antitumor activity of the conjugates was examined using mice bearing the sarcoma 180 tumor cell line. The life spans (TIC) of the mice treated with the conjugates were higher than those treated with the free 5-FU. In addition, the synthesized conjugates showed excellent antiangiogenic activity based on an embryo chorioallantoic membrane assay.

Enzymatic Synthesis of Puerarin Glucosides Using Leuconostoc Dextransucrase

  • Ko, Jin-A;Ryu, Young Bae;Park, Tae-Soon;Jeong, Hyung Jae;Kim, Jang-Hoon;Park, Su-Jin;Kim, Joong-Su;Kim, Doman;Kim, Young-Min;Lee, Woo Song
    • Journal of Microbiology and Biotechnology
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    • 제22권9호
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    • pp.1224-1229
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    • 2012
  • Puerarin (P), an isoflavone derived from kudzu roots, has strong biological activities, but its bioavailability is often limited by its low water solubility. To increase its solubility, P was glucosylated by three dextransucrases from Leuconostoc or Streptococcus species. Leuconostoc lactis EG001 dextransucrase exhibited the highest productivity of puerarin glucosides (P-Gs) among the three tested enzymes, and it primarily produced two P-Gs with a 53% yield. Their structures were identified as ${\alpha}$-$_D$-glucosyl-($1{\rightarrow}6$)-P (P-G) by using LC-MS or $^1H$- or $^{13}C$-NMR spectroscopies and ${\alpha}$-$_D$-isomaltosyl-($1{\rightarrow}6$)-P (P-IG2) by using specific enzymatic hydrolysis, and their solubilities were 15- and 202-fold higher than that of P, respectively. P-G and P-IG2 are easily applicable in the food and pharmaceutical industries as alternative functional materials.