• 제목/요약/키워드: Solution NMR

검색결과 565건 처리시간 0.031초

생체적합성과 생분해성을 갖는 키틴유도체의 합성 및 물성 III -에스테르 키틴 유도체의 합성과 용해 특성- (Synthesis and Physical Properties of Biocompatible and Biodegradable Chitin Derivatives III. -Synthesis and Solubility of Ester Chitin Derivatives-)

  • 김선정;이영무;성용길;강인규;박영훈
    • 공업화학
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    • 제4권4호
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    • pp.785-790
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    • 1993
  • 키틴의 글루코오스 단위에 메탄술폰산 존재하에서 아세트산 무수물, 프로피온산 무수물과 n-부틸산 무수물을 반응시켜 아세틸 키틴(AC), 프로피오닐 키틴(PC) 그리고 n-부티릴 키틴(BC) 등의 에스테르 형태를 갖는 개질화 키틴을 합성하였고 이들의 구조를 FT-IR과 solid state CP/MAS $^{13}C-NMR$ spectra로 확인하였다. 에스테르 형태의 키틴유도체는 대체로 키틴의 글루코오스 단위의 6번 탄소위치에 치환되었다. 유도체를 유기용매와 수용성 약산 유기용매에서 용해성을 검토하여 포름산에서 세 가지 유도체 모두 좋은 용해성을 나타냈고, 수용성 약산에서는 대부분의 유도체는 팽윤되는 것을 고찰할 수 있었다.

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Mn(Ⅲ) Chloro-Salen형 리간드 착물의 합성과 특성 (Synthesis and Characterization of Mn(Ⅲ) Chloro Complexes with Salen-Type Ligands)

  • 변종철;한충훈;박유철;이남호;백종석
    • 대한화학회지
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    • 제46권3호
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    • pp.194-204
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    • 2002
  • Cl- 이온을 포함하는 일련의 salen형 착물 {[Mn(III)($L_{acn}$)CI]: n=1~11} 들은 $Mn(CH_3COO)_2{\cdot}4H_2O$와 네자리 칸막이 리간드 {$H_2L_{acn}$}로 부터 얻었다. 이 salen형 리간드는 diamine류 {ethylenediamine, 1,3-propnediamine, 2,2-dimethyl-1,3-propanediamine, o-phenylenediamine}와 aldehyde류 {salicylaldehyde, 5-chlorosalicyladehyde, 3,5-dichlorosalicyladehyde, 3,5-di-tert-butyl-2-hydroxybenzaldehyde}를 lmethanol 용액에서 축합반응시켜 합성하였다. 이들 리간드 및 착물들은 원소 분석, 전도도, 열분석법 및 UV-VIS IR, NMR 분광학법 등을 이용하여 확인 고찰하였다.

Macrocyclic Isomers with S2O-Donor Set as Silver(I) Ionophores

  • Park, Sung-Bae;Yoon, Il;Seo, Joo-beom;Kim, Hyun-Jee;Kim, Jae-Sang;Lee, Shim-Sung
    • Bulletin of the Korean Chemical Society
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    • 제27권5호
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    • pp.713-717
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    • 2006
  • $S_2O$-donor macrocyclic isomers incorporating a xylyl group in o- ($L^1$), m- ($L^2$) and p-positions ($L^3$) extract no metal ions except silver(I) from aqueous to chloroform phase. And the magnitudes of %Ex for silver(I) are in the order of $L^1$ > $L^2$ > $L^3$. Taking this result into account, $L^1$-$L^3$ were utilized as membrane active components to prepare potentiometric silver(I)-selective electrodes. The proposed macrocycles-based electrodes E1 ($L^1$), E2 ($L^2$) and E3 ($L^3$) exhibited comparable results which show considerable selectivity toward silver(I) over alkali, alkali earth and other transition metal ions. Comparative NMR study on $L^1$-$L^3$ and their complexes with silver(I) in solution was also accomplished. In addition, a unique sandwich-type complex $[Ag(L^1)_2]CIO_4$ was prepared from the assembly reaction of $L^1$ with $AgClO_4$ and structurally characterized by an X-ray diffraction analysis.

폴리(비닐 아세테이트)의 산촉매 가수분해 반응 (Acid-Catalyzed Hydrolysis Reaction of Poly(vinyl acetate))

  • 박상수;윤희숙
    • 폴리머
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    • 제29권3호
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    • pp.304-307
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    • 2005
  • 산을 촉매로 한 물/초산용액에서의 폴리(비닐 아세테이트) 가수분해반응을 $35^{circ}C$에서, 물과 초산치 비율을 달리한 두 용액 조성에서 연구하였다. 반응시간에 따른 비닐 아세테이트(VAc)와 비닐 알코올(VA) 단량체 몰분율을 NMR로 측정하였고, 반응이 평형에 도달한 후의 화학평형상수($K_{eq}$)를 화학평형상태에서의 VAc와 VA의 몰분율을 이용하여 결정하였다. 화학평형에서의 VAc 몰분율이 0.78(${\pm}0.01$)이었을 때 $K_{ef}$는 0.76(${\pm}0.01$)이었고, VAc 몰분율이 0.57(${\pm}0.02$)일 때 0.69($\{pm}0.01$)이었다. 가수분해반응은 가성 1차 반응을 따랐으며, 반응속도상수는 $3.4{\times}10^{-6}/sec$이었다.

Structural characterization of calmodulin like domain of ryanodine receptor type 1

  • Song, Yonghyun;Kang, Sunmi;Park, Sunghyouk
    • 한국자기공명학회논문지
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    • 제19권2호
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    • pp.74-82
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    • 2015
  • Ryanodine receptor (RyR) is one of the two major $Ca^{2+}$ channels in membranes of intracellular $Ca^{2+}$ stores and is found in sarcoplasmic reticulum (SR), endoplasmic reticulum (ER). RyR1 is also the major calmodulin-binding protein of sarcoplasmic reticulum membranes. Residues 4064-4210 in the RyR1 polypeptide chain has similar primary sequence with calmodulin (CaM) and was designated as CaM-like domain (CaMLD). When expressed as a recombinant peptide, CaMLD showed several CaM-like properties in previous studies. Still, previous studies of CaMLD were focused on protein-protein interactions rather than its own properties. Here, we studied the expression of CaMLD and its sub-domains corresponding to each lobe of CaM in Escherichia coli. CaMLD could be obtained only as inclusion body, and it was refolded using urea solubilization followed by dialysis. Using spectroscopic approaches, such as NMR, circular dichroism, and gel filtration experiment, we found that the refolded CaMLD exists as nonspecific aggregate, even though it has alpha helical secondary structure. In comparison, the first half of CaMLD (R4061-4141) could be obtained as natively soluble protein with thioredoxin fusion. After the removal of the fusion tag, it exhibited folded and helical properties as shown by NMR and circular dichroism experiments. Its oligomeric status was different from CaMLD, existing as dimeric form in solution. However, the second half of the protein could not be obtained as soluble protein regardless of fusion tag. Based on these results, we believe that CaMLD, although similar to CaM in sequence, has quite different physicochemical properties and that the second half of the protein renders it the aggregative properties.

알칼리 활성반응을 이용한 플라이 애쉬/슬래그 시멘트 개발(2) - 반응생성물과 미세구조 - (Development of Fly Ash/slag Cement Using Alkali-activated Reaction(2) - Reaction products and microstructure -)

  • 박상숙;강화영;한관수
    • 대한환경공학회지
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    • 제29권7호
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    • pp.810-819
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    • 2007
  • 물유리와 수산화나트륨 용액을 이용하여 플라이 애쉬와 고로슬래그의 알칼리 활성에 관한 연구를 수행하였다. 플라이 애쉬/슬래그 시멘트 페이스트(FSC)의 반응생성물과 미세구조를 관찰하기 위하여 XRD, FTIR, $^{29}Si$ and $^{27}Al$ NMR, TGA and SEM 분석을 수행하였다. 무정형 상태 또는 저급 결정구조를 가진 calcium silicate hydrate와 aluminosilicate 겔이 각각 고로슬래그와 플라이 애쉬의 알칼리 활성반응에 의해 생성되었다. 실험결과, 물유리 모듈 1.0과 1.2가 플라이 애쉬와 고로슬래그의 알칼리 활성반응을 위해 적정한 것으로 나타났다. 물유리 모듈 1.0과 1.2로 알칼리 활성화된 FSC 페이스트는 플라이 애쉬와 고로슬래그의 알칼리 활성반응에 의해 생성된 겔 형태의 반응생성물과 물유리에 의한 또 다른 수화물(즉 실리카겔)에 의해 좀 더 단단하고 연속적이 모체가 형성되었음을 보여주었다.

고감도 수용체에 의한 ClO4- 검출 : 수용액에서 주-객 이온간의 평형 (Detection of ClO4- via A Hypersensitive Receptor : Unusual Electrostatic Equilibria between Host and Guest in Aqueous Media)

  • 이영아;홍종기;정옥상
    • 분석과학
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    • 제15권1호
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    • pp.31-35
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    • 2002
  • ${CIO_4}^-$ 이온만을 선택적으로 감지하는 새로운 수용체가 개발되었다. $[Pd(Me_4en)(Py_2S){\cdot}2ClO_4]_4$ ($Me_4en$ = N,N,N'N'-tetraethylethylenediamine; $Py_2S$ = 4,4'-dipyridyl sulfide) 착화합물에서 주-객 화학종 간의 고감도 작용력을 연구하였다. $Py_2S$의 피리딜 기는 온도, 농도, 매개체 등에 아주 민감한 두 가지의 셋트의 $^1H$ NMR, 공명 시그날을 보여주었다. 이러한 NMR 거동을 수용액에서 고리 사합체의 양이온과 ${CIO_4}^-$ 음이온 간의 정기적 인력에 의한 평형 때문인 것으로 해석되었다.

An Antifungal Antibiotic Purified from Bacillus megaterium KL39, a Biocontrol Agent of Red-Pepper Phytophthora-Blight Disease

  • JUNG HEE KYOUNG;KIM SANG-DAL
    • Journal of Microbiology and Biotechnology
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    • 제15권5호
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    • pp.1001-1010
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    • 2005
  • Bacillus megaterium KL39, an antibiotic-producing plant growth promoting rhizobacterium (PGPR), was selected from soil. The antifungal antibiotic, denoted KL39, was purified from culture filtrate by column chromatography using Dion HP-20, Silica gel, Sephadex LH-20, and prep-HPLC. Thin layer chromatography, employing the solvent system of ethanol:ammonia:water=8:1:1, showed the $R_{f}$. value of 0.32. The antibiotic KL39 showed a negative reaction with ninhydrin solution, positive with iodine vapor, and also positive with Ehrlich reagent. It was soluble in methanol, ethanol, butanol, and acetonitrile, but insoluble in chloroform, toluene, hexane, ethyl ether, or acetone. Its UV spectrum had the maximum absorption at 208 nm. Amino acid composition, FAB-mass, $^{1}H-NMR,\;^{13}C-NMR$, and atomic analyses showed that the antibiotic KL39 (MW=1,071) has a structure very similar to iturin E. The antibiotic KL39 has a broad antifungal spectrum against a variety of plant pathogenic fungi including Rhizoctonia solani, Pyricularia oryzae, Monilinia froeticola, Botrytis cinenea, Altenaria kikuchiana, Fusarium oxysporum, and F. solani. An MIC value of $10\;{\mu}g/ml$ was determined for Phytophthora capsici. Macromolecular incorporation studies with P. capsici using radioactive [$^{3}H-adenine$] as the precursor, indicated that the antibiotic KL39 strongly inhibits the DNA biosynthesis of the fungal cell. Microscopic observation of the antifungal action showed abnormal hyphal swelling of P. capsici. The purified antibiotic KL39 was very effective for the biocontrol of in vivo Phytophthora-blight disease of pepper.

PTMSP-PEI와 PDMS-PEI 복합막에 의한 수소/질소 혼합기체 분리 (Separation of $H_2$/$N_2$ Gas Mixture by PTMSP-PEI and PDMS-PEI Composite Membranes)

  • 강태범;조성혜;이현경
    • 멤브레인
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    • 제13권4호
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    • pp.291-299
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    • 2003
  • PTMSP-PEI와 PDMS-PEI 복합막을 제조하고, 막의 특성을 FT-IR, $^1H-NMR,$ DSC, TGA, GPC, SEM을 사용하여 조사하였다. 제조된 PTMSP의 수평균분자량 (equation omitted)은 477,920 이었고, 중량평균분자량 (equation omitted)은 673,329이었고, 유리전이온도 ($T_g$)는 $224^{\circ}C$이었다. 제조된 고분자 복합막들에 의한 $H_2/N_2$ 혼합기체분리는 $25^{\circ}C$에서 압력의 변화에 따라 조사되었다. PTMSP-PEI와 PDMS-PEI 복합막들의 수소에 대한 분리인자 (${\alpha}, {\beta},$ equation omitted)값은 투과셀의 압력이 증가하면 증가하였다. PTMSP-PEI 복합막의 수소에 대한 (${\alpha}, {\beta},$ equation omitted 값은 ${\Delta}P$ 30psi 와 $25^{\circ}C$에서 2.28, 1.17, 1.96이었고, PDMS-PEI 복합막의 (${\alpha}, {\beta}$ equation omitted 값은 3.70, 1.53, 2.42 이었다.

DIS 공정에 의한 Polyethylene Glycol 함침 알로에 베라 겔의 제조 및 특성화 (Preparation and Characterization of PEG-impregnated Aloe Gel through DIS Processing of Aloe vera Leaf Slice)

  • 권혜미;허원;이신영
    • KSBB Journal
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    • 제28권6호
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    • pp.356-365
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    • 2013
  • The novel Aloe gels were prepared with dewatering and impregnation by soaking (DIS) processing of Aloe vera leaf slice at four different temperatures (25, 35, 45 and $55^{\circ}C$), using dehydration solution of 40% (w/v) polyethylene glycol (PEG4000). The PEG-impregnation to Aloe vera leaf slice during DIS was observed depending on immersion temperature, and the PEG-impregnated Aloe vera gel (PEG-i-AVG) obtained was characterized using $^1H$ NMR, FT-IR, GPC, XRD and TGA. The PEG-i-AVG had the higher levels of Aloe bioactives (glucomannan and O-acetyl contents) and better quality indices by $^1H$ NMR and FT-IR spectroscopy than those of native Aloe gel. Also, the obtained Aloe gel maintained the bimodal patterns in higher molecular weight region by GPC indicating no degradation of polysaccharide from native Aloe gel. The result observed by SEM confirmed a surface modification by forming the porous structure, and TGA result exhibited better thermal stability than that of native Aloe gel. XRD result revealed that the crystalline structure in Aloe gel was led by incorporation of PEG. Significant decrease of %insolubility and high enhancement of water solubility index were observed, respectively, and highly ordered conformation such as a helix structure was also indicated by Congo red reaction. We concluded that the modification effect for enhancing function of native Aloe gel was successfully obtained by DIS process using PEG as a dehydrating agent. These results suggested that this DIS process had a high potential for developing a new minimally processed product from Aloe vera leaf.