• 제목/요약/키워드: 2 D-NMR

검색결과 1,009건 처리시간 0.028초

Successive Synthesis of Well-Defined Star-Branched Polymers by an Iterative Approach Based on Living Anionic Polymerization

  • Higashihara Tomoya;Inoue Kyoichi;Nagura Masato;Hirao Akira
    • Macromolecular Research
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    • 제14권3호
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    • pp.287-299
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    • 2006
  • To successively synthesize star-branched polymers, we developed a new iterative methodology which involves only two sets of the reactions in each iterative process: (a) an addition reaction of DPE or DPE-functionalized polymer to a living anionic polymer, and (b) an in-situ reaction of 1-(4-(4-bromobutyl)phenyl)-1-phenylethylene with the generated 1,1-diphenylalkyl anion to introduce one DPE functionality. With this methodology, 3-, 4-, and 5-arm, regular star-branched polystyrenes, as well as 3-arm ABC, 4-arm ABCD, and a new 5-arm ABCDE, asymmetric star-branched polymers, were successively synthesized. The A, B, C, D, and E arm segments were poly(4-trimethylsilylstyrene), poly(4-methoxystyrene), poly(4-methylstyrene), polystyrene, and poly(4-tert-butyldimethylsilyloxystyrene), respectively. All of the resulting star-branched polymers were well-defined in architecture and precisely controlled in chain length, as confirmed by SEC, $^1H$ NMR, VPO, and SLS analyses. Furthermore, we extended the iterative methodology by the use of a new functionalized DPE derivative, 1-(3-chloromethylphenyl)-1-((3-(1-phonyletheny1)phenyl) ethylene, capable of introducing two DPE functionalities via one DPE anion reaction site in the reaction (b). The number of arm segments of the star-branched polymer synthesized by the methodology could be dramatically increased to 2, 6, and up to 14 by repeating the iterative process.

68 cm 상온 보아를 갖는 MRI용 초전도마그네트에 관한 연구 (The Study on the Superconducting MRI Magnet of 68 cm in Room Temperature Bore)

  • 진흥범;오봉환;조전욱;오상수;권영길;하동우;이언용;김해종;김옥곤;최병주;류강식
    • 대한의용생체공학회:학술대회논문집
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    • 대한의용생체공학회 1996년도 추계학술대회
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    • pp.142-146
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    • 1996
  • In this paper, we present the main research results on the 2 Tesla class - superconducting MRI magnet which we have developed. Multi section type superconducting MRI main coil and various superconducting shims were designed and fabricated for obtaining the high field homogeneity, which is requested in the MR imaging. After assembling the magnet with room temperature bore cryostat field homogenity has been measured and analyzed by NMR field mapping system. According to this, field homogeneity of 22 ppm / 30 cm dsv was confirmed.

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수종 복합레진 내의 bis-GMA와 TEGDMA의 구성비가 레진 인레이 법에 의한 부가적 열처리시 복합레진의 표면 및 내부의 중합률 변화에 미치는 영향 (CORRELATION BETWEEN BIS-GMA : TEGDMA RATIO AND DEGREE OF CONVERSION IN VARIOUS LAYERS OF COMPOSITE AFTER ADDITIONAL HEAT CURING)

  • 박성호;정찬문
    • Restorative Dentistry and Endodontics
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    • 제21권2호
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    • pp.642-651
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    • 1996
  • The purpose of this study was to evaluate the relationship between monomer compositions and the changes in the degree of conversion in the various layers of composites after additional heat curing. Four types of composites and 3 types of inlay ovens were used in this study. Composite was placed in a 4-mm thick teflon mold, and light cured from the top for 60 seconds. Ten samples were prepared for each composite ; 5 of these were additionally heat cured in an inlay oven as the manufacturer recommended. After light curing or light and heat curing, the samples were sectioned into four parts and assigned to groups A, B, C, or D according to their distance from the light source. These sections were then thinned to 50-$70{\mu}m$, and these wafers were analyzed with a Fourier Transform Infrared Spectrometer(FI-IR) to determine the degree of conversion. A standard baseline technique was used to calculate the degree of conversion. $^{13}C$ NMR spectra of bis-GMA, TEGDMA and bis-EMA, were acquired using a Varian Gemini spectrometer operated at 200 MHz. $CDCl_3$ solvent was used for qualitative analysis. The degree of conversion was affected by bis-GMA : TEGDMA ratio but it seemed to be also affected by other factors. When the composites were heat cured, significant increases in the degree of conversion were noted throughout the samples, but the amount of increase differed between materials. Thus, clinical performance of a heat-treated composite inlay may be different depending on materials.

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Sesquiterpenoids from the Stem Bark of Aglaia grandis

  • Harneti, Desi;Permatasari, Atika Ayu;Anisshabira, Amallya;Naini, Al Arofatus;Nurlelasari, Nurlelasari;Mayanti, Tri;Maharani, Rani;Safari, Agus;Hidayat, Ace Tatang;Farabi, Kindi;Supratman, Unang;Azmi, Mohamad Nurul;Shiono, Yoshihito
    • Natural Product Sciences
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    • 제28권1호
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    • pp.6-12
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    • 2022
  • Five sesquiterpenoids, 7-epi-eudesm-4(15)-ene,1β,6α-diol (1), 7-epi-eudesm-4(15)-ene,1β,6α-diol (2), saniculamoid D (3), aphanamol I (4), and 4β,10α-dihydroxyaromadendrane (5), were isolated from the stem bark of Aglaia grandis. The compounds' (1-5) chemical structures were identified by spectroscopic data including, IR, NMR (1H, 13C, DEPT 135°, HMQC, HMBC, 1H-1H COSY), and HRTOFMS, as well as by comparing with the previously reported spectral data. Therefore, this study described the structural elucidation of compounds 1-5 and evaluated their cytotoxic effects against Hela cervical and B16F10 melanoma cells for the first time, but no significant result was discovered.

식용식물자원으로부터 활성물질의 탐색-XXII. 사자발쑥(Artemisia princeps PAMPANINI)의 지상부로부터 Triterpenoid의 분리 (Development of Biologically Active Compounds from Edible Plant Sources XXII. Triterpenoids from the Aerial Parts of Sajabalssuk (Artemisia princeps PAMPANINI))

  • 방면호;조진경;송명종;이대영;한민우;정해곤;정태숙;이경태;최명숙;백남인
    • Applied Biological Chemistry
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    • 제51권3호
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    • pp.223-227
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    • 2008
  • 사자발쑥의 지상부를 80% MeOH용액으로 추출하고, 얻어진 추출물을 EtOAc, H-BuOH 및 $H_2O$로 용매 분획 하였다. 이 중 EtOAc 분획으로부터 silica gel과 octadecyl silica gel(ODS), Sephadex LH-20 column chromatography로 정제하여 4종의 triterpenoid를 분리하였다. 각 화합물의 화학구조는 NMR, MS 및 IR 등의 스펙트럼 데이터를 해석하여 wrightial(1), wrightial acetate(2), 27-norcycloart-20(21)-ene-25-al-3${\beta}$-ol acetate(3) 및 ursolic acid(4)로 동정하였다. 이 화합물들은 사자발쑥에서 처음으로 분리 보고 되었으며 특히, 화합물 3은 천연에서 처음으로 분리 보고 되었다. 또한 이번에 분리한 화합물에 대하여 항고지혈증 활성을 측정한 결과 화합물 1은 ACAT1과 ACAT2 효소에 대한 $IC_{50}$ 값이 33 ${\mu}g/ml$와 45 ${\mu}g/ml$로 나타났고, 화합물 2는 ACAT1 효소에 대하여 $IC_{50}$ 값이 12 ${\mu}g/ml$로 나타났다. 화합물 3은 ACATI 효소에 대하여 $IC_{50}$값이 16 ${\mu}g/ml$으로 나타났다.

New hydroperoxylated and 20,24-epoxylated dammarane triterpenes from the rot roots of Panax notoginseng

  • Shang, Jia-Huan;Sun, Wen-Jie;Zhu, Hong-Tao;Wang, Dong;Yang, Chong-Ren;Zhang, Ying-Jun
    • Journal of Ginseng Research
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    • 제44권3호
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    • pp.405-412
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    • 2020
  • Background: Root rot is a serious destructive disease of Panax notoginseng, a famous cultivated araliaceous herb called Sanqi or Tianqi in Southwest China. Methods: The chemical substances of Sanqi rot roots were explored by chromatographic techniques. MS, 1D/2D-NMR, and single crystal X-ray diffraction were applied to determine the structures. Murine macrophage RAW264.7 and five human cancer cell lines were used separately for evaluating the antiinflammatory and cytotoxic activities. Results and Conclusion: Thirty dammarane-type triterpenes and saponins were isolated from the rot roots of P. notoginseng. Among them, seven triterpenes, namely, 20(S)-dammar-25-ene-24(S)-hydroperoxyl-3β,6α,12β,20-tetrol (1), 20(S)-dammar-3-oxo-23-ene-25-hydroperoxyl-6α,12β,20-triol (2), 20(S)-dammar-12-oxo-23-ene-25-hydroperoxyl-3β,6α,20-triol (3), 20(S)-dammar-3-oxo-23-ene-25-hydroperoxyl-12β,20-diol (4), 20(S),24(R)-epoxy-3,4-seco-dammar-25-hydroxy-12-one-3-oic acid (5), 20(S),24(R)-epoxy-3,4-seco-dammar-25-hydroxy-12-one-3-oic acid methyl ester (6), and 6α-hydroxy-22,23,24,25,26,27-hexanordammar-3,12,20-trione (7), are new compounds. In addition, 12 known ones (12-16 and 19-25) were reported in Sanqi for the first time. The new Compound 1 showed comparable antiinflammatory activity on inhibition of NO production to the positive control, whereas the known compounds 9, 12, 13, and 16 displayed moderate cytotoxicities against five human cancer cell lines. The results will provide scientific basis for understanding the chemical constituents of Sanqi rot roots and new candidates for searching antiinflammatory and antitumor agents.

Inhibition of Low Density Lipoprotein-oxidation, ACAT-1, and ACAT-2 by Lignans from the Bark of Machilus thunbergii

  • Shrestha, Sabina;Park, Ji-Hae;Lee, Dae-Young;Cho, Jin-Gyeong;Lee, Do-Gyeong;Cho, Moon-Hee;Jeong, Tae-Sook;Kang, Hee-Cheol;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • 제54권1호
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    • pp.63-66
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    • 2011
  • The bark of Machilus thunbergii was extracted with 80% aqueous methanol (MeOH), and the concentrated extract was partitioned using ethyl acetate (EtOAc), butanol (n-BuOH), and $H_2O$, successively. From the EtOAc fraction, five lignans were isolated through the repeated silica gel, octadecyl silica gel (ODS) and, Sephadex LH-20 column chromatography. Based on nuclear magnetic resonance (NMR), mass spectroscopy (MS), and infrared spectroscopy (IR) spectroscopic data, the chemical structures of the compounds were determined to be machilin A (1), machilin F (2), licarin A (3), nectandrin A (4), and nectandrin B, (5). This study presents comparative account of five lignans from M. thunbergii bark contributing inhibition of low density lipoprotein (LDL), ACAT-1, and ACAT-2. Compounds 2-5 showed varied degree of antioxidant activity on LDL with $IC_{50}$ values of 2.1, 11.8, 15.3, and $4.1{\mu}M$. Compounds 1, 2, and 3 showed inhibition activity on ACAT-1 with values $63.4{\pm}6.9%$ ($IC_{50}=66.8{\mu}M$), $53.7{\pm}0.9%$ ($IC_{50}=109.2{\mu}M$), and $78.7{\pm}0.2%$ ($IC_{50}=40.6{\mu}M$), respectively, at a concentration of 50 mg/mL, and on ACAT-2 with values $47.3{\pm}1.5%$ ($IC_{50}=149.7{\mu}M$), $39.2{\pm}0.2%$ ($IC_{50}=165.2{\mu}M$), and $52.1{\pm}1.0%$ ($IC_{50}=131.0{\mu}M$, respectively, at a concentration of 50 mg/mL.

Effects of Microbacterium laevaniformans Levans Molecular Weight on Cytotoxicity

  • Oh, Im-Kyung;Yoo, Sang-Ho;Bae, In-Young;Cha, Jae-Ho;Lee, Hyeon-Gyu
    • Journal of Microbiology and Biotechnology
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    • 제14권5호
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    • pp.985-990
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    • 2004
  • Levans produced from Microbacterium laevaniformans were isolated, characterized, and fractionated by molecular weight. TLC, HPLC, and GC-MS analyses of the exopolysaccharide showed that it was a fructan-type polymer and was composed of (2,6)- and (2,1)-glycosidic linkages. $^{13}C$-NMR analysis proved that the polysaccharide was mainly a $\beta$-(2,6)-linked levan-type polysaccharide. To investigate the cytotoxicity of the acetone-precipitated levan fractions such as M1, M2, and M3, HepG2, P388D1, U937, SNU-1, and SNUC2A cell lines were screened. Among the cell lines tested, the cytotoxicity of M1- M3 fractions were detected from only SNU-1 and HepG2 cells at the dosage level of $100-800\mu\textrm{g}ml$. The M2 fraction M_r$, 80,000) at 400 $mu{g/ml}$ had the greatest cell growth inhibition (84.6%) on SNU-1, while the M1 $(M_r$, 50,000) at $800\mu\textrm{g}ml$ showed the greatest (46.32%) on HepG2. To obtain more uniform M_r$ fractions of levan, the levan was further fractionated from S1 $(M_r$ 1,000,000) to S5 $(M_r$ 10,000) using gel permeation chromatography. Again, the S1-S5 fractions had strong cytotoxicity on SNU-1 and HepG2 cell lines. The greatest inhibition effects of S4 $(M_r$ 80,000) on SNU-1 and S5 $(M_r$ 10,000) on HepG2 were shown to be 49.5% and 73.0%, respectively. The cytotoxicity of the levan fractions was more effective on SNU-1 than on HepG2. Although the relationship between the Mw and the cytotoxicity was not clear, smaller $M_r$, fractions of levan showed greater growth inhibition effect on the cancer cell lines in general. Therefore, it was indicated that a specific Mw class of levan is responsible for the effective cytotoxicity.

Copolymerization of Ethylene and Norbornene via Polymethylene Bridged Dinuclear Constrained Geometry Catalysts

  • Zhu, Yin-Bang;Jeong, Eung-Yeong;Lee, Bae-Wook;Kim, Bong-Shik;Noh, Seok-Kyun;Lyoo, Won-Seok;Lee, Dong-Ho;Kim, Yong-Man
    • Macromolecular Research
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    • 제15권5호
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    • pp.430-436
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    • 2007
  • The dinuclear half-sandwich CGCs (constrained geometry catalyst) with a polymethylene bridge, $[Ti({\eta}^5 : {\eta}^1-indenyl)SiMe_2NCMe_3]_2(CH_2)_n]$[n = 6 (1) and 12 (2)], have been employed in the copolymerization of ethylene and norbornene (NBE). To compare the mononuclear metallocene catalysts; $Ti({\eta}^5 : {\eta}^1-2-hexylindenyl)SiMe_2NCMe_3$ (3), $(Cp^* SiMe_2NCMe_3)$Ti (Dow CGC) (4) and ansa-$Et(Ind)_2ZrCI_2$ (5), were also studied for the copolymerization of ethylene and NBE. It was found that the activity increased in the order: 1 < 2 < 3 < 5 < 4, indicating that the presence of the bridge between two the CGC units contributed to depressing the polymerization activity of the CGCs. This result strongly suggests that the implication of steric disturbance due to the presence of the bridge may playa significant role in slowing the activity. Dinuclear CGCs have been found to be very efficient for the incorporation of NBE onto the polyethylene backbone. The NBE contents in the copolymers formed ranged from 10 to 42%, depending on the polymerization conditions. Strong chemical shifts were observed at ${\delta}$42.0 and 47.8 of the isotactic alternating NBE sequences, NENEN, in the copolymers with high NBE contents. In addition, a resonance at 47.1 ppm for the sequences of the isolated NBE, EENEE, was observed in the $^{13}C-NMR$ spectra of the copolymers with low NBE contents. The absence of signals for isotactic dyad at 48.1 and 49.1 ppm illustrated there were no isotactic or microblock (NBE-NBE) sequences in the copolymers. This result indicated that the dinuclear CGCs were effective for making randomly distributed ethylene-NBE copolymers.

분자생물학적 TMV 및 PVY 저항성 연초 육종 (Molecular Breeding of Tobacco Plants Resistant to TMV and PVY)

  • E.K. Pank;Kim, Y.H.;Kim, S.S.;Park, S.W.;Lee, C.H.;K.H.Paik
    • 한국연초학회:학술대회논문집
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    • 한국연초학회 1997년도 담배과학 국제학술대회
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    • pp.134-152
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    • 1997
  • 담배 모자이크 바이러스(TMV)와 감자 바이러스 Y(PVY) 등 식물바이러스병은 잎담배 생산에 심한 경제적 손실을 초래하고 있다. 바이러스병 방제를 위한 여러 가지 경종적 방법은 충분한-방제 효과를 얻지 못하는 경우가 많아 바이러스의 방제에는 우수한 저항성 품종의 사용이 가장 바람직한 것으로 알려져 있다. 그러나 기존의 육종 방법이 저항성 품종 개발에 항상 바람직한 것은 아닌데 그 이유는 저항성 유전자원이 없는 경우가 많고 또한 육종을 통해 유전자원의 열등한 특성이 도입될 수 있기 때문이다. 따라서 본 연구실에서는 TMV와 PVY의 여러 가지 형태의 외피단백질(CP) (비전사부분 포함 또는 제거, 비 전사부분 등) 및 복제유전자(Nlb) (3' 및 5' 결손 유무, 돌연변이)를 상용 담배 품종인 NC 82와 Burley 21에 형질전환시켜 바이러스 저항성 개발을 시도하였다. 각각의 유전자 cDNA를 1-2개의 35S promotor를 가진 식물발현벡타에 클로닝한 후 Agrobacteriupn (upnefaciens LBA 4404를 이용하여 식물의 잎조직에 도입시킨 후 kanamycin 함유 MS 배지에서 식물체를 재닥화하였다. 재분화 식물체는 TMV와 PVY에 대한 저항성 검정을 하였다. 그 결과 TMV에 저항성인 TMV CP 형질전환 식물체와 8 가지 Nlb 형질전환 식물체 계통 중에 6 계통의 저항성 형질전환 식물체를 획득하였다. 여기에서는 TMV와 PVY의 접종시험을 통하여 각각의 바이러스에 대한 형질전환 담배의 계통별 저항성 정도를 조사하고, 저항성 형질전환 식물체에서의 도입 유전자 확인하며, 세대별 저항성의 유전 및 안정성을 살펴보고자 한다. 또한 유망 저항성 형질전환 계통의 식물체 내에서의 바이러스 증식 및 이동과 관련된 저항성 기작, 여러 가지 PVY 계통에 대한 저항성 유무, 수량, 생육 특성 및 주요 화학 성분 함량 등을 발표하고자 한다.-glucose로 구성된 다당류 이었다. 아미노산은 Asp 및 Glu의 산성 아미노산과 Ala, Leu 등의 함량이 높게 나타났으며, 비알칼리 추출물에서 Ser과 Thr의 함량이 높게 나타났다. 다당류 T-AS는 평균 분자량이 2,000 kD와 12kD에서 주 peak를 나타냈으며, 수용성 분획의 평균 분자량은 12kD이고 비수용성 분획은 36~2,000 kD의 평균 분자량 분포를 갖는 것으로 나타났다. IR과 NMR 분석 결과 890 cm-1에서 흡수 peak를 나타내어 $\beta$-(1,3)0glucan과 $\beta$-(1,6)-glucan의 구조를 갖는 다당류로 확인 되었다. T-AS 분획은 C:H:O:N의 함량비가 38.9:5.7:49.6:1.84%이며, 이 물질의 융점은 163 $^{\circ}C$로 연한 갈색을 나타낸다. 분리된 GLG의 항암활성 기전 규명을 위해, in vivo 항암실험, 항보체 활성능, 항체 생성능, serum protein 분비능, 대식세포의 탐식능과 활성능 및 세포간 물질 분비 등의 상관관계를 조사하였다. 다당류 GLG 분획물들 가운데 항보체의 활성이 높았던 분획은 sarcome 180에 대한 항암 활성이 높게 나타났다. 다당류 T-AS의 보체 활성화 기작은 classical과 alternative complement pathway의 양 경로를 통해 활성화 되었다. T-AS 분획은 mouse내의 특정 혈청단백을 증가시켰으며, 항체 생성능의 증가가 관찰되어 effect T 세포의 활성화가 나타나고 있음을 알 수 있었다. T-AS는 생체내 투여시에 대식세포의 탐식능이 증진되었으며, 대식세포 기능 저해제에 의한 대식세포의 기능 저해 현상이 회복되었다. 이와 같은 결과들로부터, T-AS의 항암 활성은 활성화된 보체 성분 및 당 수용체들이 존재하는 대식세포의 개입을 시사한다.가능성과

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