• 제목/요약/키워드: $^{1}H$ NMR

검색결과 2,519건 처리시간 0.03초

계면활성제 수용액에서 미셀형성(제2보) - 계면활성제/탄화수소/물의 상 변화에 따른 자기확산 - (Studies on the Micelle Formation of Surfactant Solution(2) - Self-Diffusion by Phase Transition in Ternary System of Surfactant/Hydrocarbon/Water -)

  • 최성옥;이진희;김상춘;남기대
    • 공업화학
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    • 제10권1호
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    • pp.112-117
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    • 1999
  • Pulsed Field Gradient NMR(FT-PFGE)을 이용하여 N-alkyl-N, N-dimethylamine oxide/hydrocarbon/$D_2O[C_nDMAO/C_{n^{\prime}}H_{{2n^{\prime}+2}}/D_2O]$ 3성분 계에서 자기확산 계수를 측정하였다. 여기서 n = 12, 14, 16인 계면활성제를 사용하였으며, n' = 6, 8, 10, 12, 14인 탄화수소를 사용하였다. 미셀 상에서 주로 확산은 미셀의 유체역학적 이동에 지배되며, 미셀들의 충돌로 가용화된 탄화수소의 교환에 의해서도 일부 이루어진다. 이 연구는 계면활성제의 알킬 사슬 길이와 탄화수소 분자크기의 변화에 따라서 검토되었다. 그 결과 큐빅 상에서 용매는 물의 연속상에서 거동에 대한 전형적인 자기확산 계수 값을 나타내고, 이때 장애물로서 마이크로에멀젼 액적이 작용한다. 겔 상태에서 계면활성제의 유동성은 낮고, 알킬 사슬 길이가 가장 짧은 계면활성제에 대해서만 결정되었다. 겔 내에서 미셀들 간의 탄화수소 교환은 호핑 과정에 의해서 일어나는 것을 알았고, 회합율은 계면활성제의 알킬 사슬 길이에 따라 감소하였다.

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식용식물자원으로부터 활성물질의 탐색-XIV. 사자발쑥(Artemisia herba)의 전초로부터 flavonoid 화합물의 분리 (Development of Biologically Active Compounds from Edible Plant Sources XIV. Isolation and Identification of Flavonoids from the Aerial Parts of Sajabalssuk (Artemisia herba))

  • 방면호;김동현;유종수;이대영;송명종;양혜정;정태숙;이경태;최명숙;정해곤;백남인
    • Applied Biological Chemistry
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    • 제48권4호
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    • pp.418-420
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    • 2005
  • 사자발쑥의 전초를 80% MeOH 용액으로 추출하고, 추출물을 EtOAc, n-BuOH 및 물로 분배, 추출하였다. 이 중 EtOAc 분획을 silica gel과 octadecylsilica gel(ODS) column chromatography로 정제하여 4종의 화합물을 분리하였다. 각 화합물의 화학구조는 NMR, MS 및 IR 등의 스펙트럼 데이터를 해석하여, eupatilin (1), jaceosidin (2), apigenin (3) 및 eupafolin (4)으로 동정하였다. 이들 중 eupatilin과 jaceosidin은 사자발쑥에서 분리, 보고 된 바 있으나 eupafolin과 apigenin은 처음 분리되었다.

Mutant Recombinant Hemoglobin (${\alpha}96Val{\rightarrow}Tyr$) Exhibits Low Oxygen Affinity and High Cooperativity

  • Choi, Jong-Whan;Yeh, Byung-Il;Han, Dong-Pyou;Lee, Hyean-Woo;Sohn, Joon Hyung;Jung, Seun-Ho;Kim, Hyun-Won
    • BMB Reports
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    • 제31권6호
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    • pp.595-599
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    • 1998
  • To investigate conformational information of a low oxygen affinity recombinant hemoglobin (rHb) containing $96Val{\rightarrow}Trp$ mutation at the ${\alpha}96$ position, we ave produced rHb (${\alpha}96Val{\rightarrow}Phe$) and rHb (${\alpha}96Val{\rightarrow}Tyr$), using the Escherichia coli expression system and site-directed mutagenesis. The oxygen affinity of rHb (${\alpha}96Val{\rightarrow}Phe$) is similar to that of human normal adult hemoglobin (Hb A). However, the oxygen affinity of rHb (${\alpha}96Val{\rightarrow}Tyr$) showed much lower oxygen affinity than Hb A which is similar to that of rHb (${\alpha}96Val{\rightarrow}Tyr$), providing an opportunity as a potential candidate for a hemoglobin-based blood substitute. Both rHb (${\alpha}96Val{\rightarrow}Phe$) and rHb (${\alpha}96Val{\rightarrow}Tyr)$ showed high cooperativity in oxygen binding. IH-NMR spectroscopy shows that both rHb (${\alpha}96Val{\rightarrow}Phe$) and rHb (${\alpha}96Val{\rightarrow}Tyr$) have very similar tertiary structure around the heme pockets and uaternary structure in the ${\alpha}_1/{\beta}_2$ subunit interface ompared to Hb A. The low oxygen affinity of rHb (${\alpha}96Val{\rightarrow}Tyr$) has been suggested to be due to a hydrogen bond caused by an extra hydroxyl group not present in rHb (${\alpha}96Val{\rightarrow}Phe$). However, investigation of the carbonmonoxy form of rHb (${\alpha}96Val{\rightarrow}Phe$) and (${\alpha}96Val{\rightarrow}Try$) in the presence of inositol hexaphosphate at low temperature suggests that low oxygen affinity of (${\alpha}96Val{\rightarrow}Try$) may arise from a mechanism different to that of rHb (${\alpha}96Val{\rightarrow}Trp$).

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식용식물자원으로부터 활성물질의 탐색 XVI. -사자발쑥(Artemisia herba)의 전초로부터 sterol 화합물의 분리- (Development of Biologically Active Compounds from Edible Plant Sources XVI. -Isolation of Sterols from the Aerial Parts of Sajabalssuk (Artemisia herba)-)

  • 방면호;정해곤;송명종;유종수;정선아;이대영;김세영;정태숙;이경태;최명숙;백남인
    • Applied Biological Chemistry
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    • 제49권2호
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    • pp.140-144
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    • 2006
  • 사자발쑥의 전초를 80% MeOH 용액으로 추출하고, 얻어진 추출물을 EtOAc, n-BuOH 및 물로 용매 분획 하였다. 이 중 EtOAc 분획과 n-BuOH 분획으로부터 silica gel과 octadecyl silica gel(ODS) column chromatography로 정제하여 4종의 sterol 화합물을 분리하였다. 각 화합물의 화학구조는 NMR, MS 및 IR 등의 스펙트림 데이터를 해석하여, ${\beta}-sitosterol$ (1), dehydroergosterol $5{\alpha},8{\alpha}-epidioxide$ (2), stigmasterol (3), daucosterol (4)으로 동정하였다. 이 화합물들은 사자발쑥에서 처음 분리되었다.

후박피(Magnoliae bark)로부터 항충치활성을 갖는 물질의 분리 (Isolation of an Anticariogenic Compound from Magnoliae Bark)

  • 이윤수;박헌주;유재선;박형환;권익부;이현용
    • 한국식품과학회지
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    • 제30권1호
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    • pp.230-236
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    • 1998
  • 충치 원인균인 S. mutans가 생산하는 불용성, 부착성 glucan 합성효소인 GTase의 활성을 저해하는 물질을 생약재로 부터 탐색, 개발하여 기능성 식품 또는 의약품의 소재로 응용하는 것을 목적으로 연구를 수행하였다. 32종의 생약재 추출물에 대하여 GTase 저해활성을 측정한 결과, 후박피에서 가장 높은 활성이 관찰되었다. 후박피 추출물에 대하여 용매분획을 행한 결과 ethylacetate층에 대부분의 활성이 존재하였으므로, 이 획분을 silicagel column chromatography, prep. HPLC 등을 이용하여 더욱 분리, 정제하여 순수한 GTase 저해물질을 분리하였다. 이 물질의 분리수율은 0.013% (w/w)였다. 이 화합물을 UV, FAB-MS 및 NMR spectrometry 등을 이용하여 화학구조의 해석을 실시한 결과 이 물질은 coniferyl alcohol의 중합체로 lignan계 화합물인 4,4'-dihydroxy-3,3'-dimethoxylignan (분자량 330)으로 확인되었다. 이 화합물은 후박피에서는 최초로 확인된 물질이다. 또한 충치 원인균인 S. mutans를 포함한 11종의 구강 미생물에 대한 항균성을 검토한 결과 비교 화합물에 비해 비교적 강력한 활성$(MIC;\;31.3\;{\mu}g/ml)$이 나타났다. 지금까지 후박피는 반하후박탕, 후박삼물탕 등 한방약재의 중요한 원료로 이용되어 왔으며, 복통의 치료효과 및 건위 작용 등이 알려져 있다. 또한 후박피 중에는 diphenyl계 화합물인 magnolol 및 honokiol등이 함유되어 있어 이들 물질이 건위작용을 돕는 것으로 알려져 있을 뿐이다. 따라서 이번에 새롭게 확인된 4,4'-dihydroxy-3,3'-dimethoxylignan이 충치 예방효과를 지니고 있다는 사실은 금후 산업적 응용면에서도 매우 중요한 결과로 여겨져 지속적인 연구가 기대된다.

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Piperlongumine 유도체 합성과 $Aflatoxin\;B_1$ 생성 억제 효과 (Synthesis of Piperlongumine Derivatives Isolated from Piper longum L. and their Inhibitory Activity on Aflatoxin $B_1$ Production)

  • 이성은;최원식;이현상;이영행;박병수
    • Applied Biological Chemistry
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    • 제46권4호
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    • pp.361-366
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    • 2003
  • 필발 열매로부터 추출 및 분리한 piperlongurnine (1-[3-(3,4,5-trimethoxyphenyl)acryloyl]-5,6-dihydro-1H-pyridin-2-one)이 aflatoxin $B_1\;(AFB_1)$ 생성억제에 있어서 탁월한 효과가 입증되어 3,4,5-trimethoxycinnamic acid (TMCA)를 모체로 하여 1-piperidin-1-yl-3-(3,4,5-trimethoxyphenyl)propenone (1), 1-morpholin-4-yl-3-(3,4,5-trimetholfrphenyl)propenone (2), 1- (3,5-dimethylpiperidin-1-yl)-3-(3,4,5-trimethoxyphenyl)propenone (3), 1-(2-methylperidin-1-yl)-3-(3,4,5-trimethoxyphenyl)propenone (4), 1- (3-hydroxypiperidin-1-yl)-3-(3,4,5-trimethoxyphenyl)propenone (5), 1-[3-(3,4,5-trimethoxy-phenyl)acryloyl]piperidin-2-one (6) 및 ethyl 1-[3-(3,4,5-trimethoxyphenyl)acryloyl]piperidin-4-carboxylate (7)의 유도체를 합성하여 구조를 확인하고, 이 화합물들을 이용하여 $AFB_1$ 생성저해 효과를 측정하였다. Aspergillus flavus NRRL 2061로부터 생성되는 $AFB_1$ 생성저해에 대한 실험한 결과 모든 유도체 화합물에서 활성을 나타내었으며, 특히 화합물 (3)이 1000, 500, 250, 100및 $50\;{\mu}g/ml$에서 100, 95, 90, 53 및 10%의 생성저해를 나타냈다. 이러한 연구 결과 유도체 화합물 (3)은 항진균 독소제 개발을 위한 선도화합물로 이용하여 새로운 농약으로 개발이 가능할 것이라고 판단된다.

Aburatubolactam C, a Novel Apoptosis-inducing Substance Produced by Marine Streptomyces sp. SCRC A-20

  • Bae, Myung-Ae;Yamada, Kaoru;Uemura, Daisuke;Seu, Jung-Hwan;Kim, Young-Ho
    • Journal of Microbiology and Biotechnology
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    • 제8권5호
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    • pp.455-460
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    • 1998
  • In the course of screening for new antitumor substances, a novel cytotoxic agent inducing apoptotic cell death was isolated from the culture broth of marine bacterial strain SCRC A-20. Strain SCRC A-20 was separated from a mollusk and was chemotaxonomically identified as a Streptomyces sp. The cytotoxic substance was purified by organic solvent extraction followed by silica gel column chromatography and preparative TLC. HRFAB-MS determined its molecular formula to be $C_{30}H_{40}N_2O_5$ (MW 508). The 1D and 2D NMR spectral data demonstrated that the substance has a novel lactam structure of a 20-membered macrocycle coupled with a unique acyl tetramine and bicyclo[3.3.0] octane, which includes three methyl groups, six olefinic protons, five carbonyl groups, a conjugated diene and a dienone. The substance, named aburatubolactam C, appeared to be cytotoxic for various continuously proliferating tumor cells of human and murine origins. The $IC_{50}$ values determined by MIT assay were in the range of 0.3 to $5.8\mug/ml$. When Jurkat T cells were treated with $3\mug/ml$. of aburatubolactam C, the apoptotic DNA fragmentation was detectable within 3 h, indicating that the cytotoxic effect of aburatubolactam C on tumor cells is attributable to the induced apoptosis.

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Ligand Binding Properties of the N-Terminal Domain of Riboflavin Synthase from Escherichia coli

  • Lee, Chan-Yong;Illarionov, Boris;Woo, Young-Eun;Kemter, Kristina;Kim, Ryu-Ryun;Eberhardt, Sabine;Cushman, Mark;Eisenreich, Wolfgang;Fischer, Markus;Bacher, Adelbert
    • BMB Reports
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    • 제40권2호
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    • pp.239-246
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    • 2007
  • Riboflavin synthase from Escherichia coli is a homotrimer of 23.4 kDa subunits and catalyzes the formation of one molecule each of riboflavin and 5-amino-6-ribitylamino- 2,4(1H,3H)-pyrimidinedione by the transfer of a 4-carbon moiety between two molecules of the substrate, 6,7- dimethyl-8-ribityllumazine. Each subunit comprises two closely similar folding domains. Recombinant expression of the N-terminal domain is known to provide a $C_2$-symmetric homodimer. In this study, the binding properties of wild type as well as two mutated proteins of N-terminal domain of riboflavin synthase with various ligands were tested. The replacement of the amino acid residue A43, located in the second shell of riboflavin synthase active center, in the recombinant N-terminal domain dimer reduces the affinity for 6,7-dimethyl-8-ribityllumazine. The mutation of the amino acid residue C48 forming part of activity cavity of the enzyme causes significant $^{19}F$ NMR chemical shift modulation of trifluoromethyl derivatives of 6,7-dimethyl-8-ribityllumazine in complex with the protein, while substitution of A43 results in smaller chemical shift changes.

경피용 프로드럭인 에칠 글리콜레이트의 국소자극 및 피부투과성 (Skin Penetration and Local Irritation of Ethyl Glycolate, a Potential Transdermal Prodrug)

  • 양성운;하용호;김종갑;최영욱
    • 약학회지
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    • 제40권2호
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    • pp.155-162
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    • 1996
  • Hyperkeratinization is a dermatologic disorder, which is due to the increase of corneocyte cohesion force. Glycolic acid, an alpha hydroxy acid(AHA), has been used to breakdown the hyperkeratinization processes. However, it has a problem of skin irritation when applied topically, due to the strong acidity especially in high concentration. A molecular optimization of glycolic acid has been tried to reduce the skin irritation by the way of prodrug formation. Ethyl glycolate was synthesized by the esterification of glycolic acid with ethanol in acidic conditions in the presence of sulfuric acid, and examined under the spectroscopic trials, such as UV, IR, $^1H$-NMR, and GC-MS. The physicochemical and biopharmaceutical properties of the prodrug were also evaluated. Through the toxicological tests of both skin irritation and eye mucous irritation, it has been proved that ethyl glycolate was less irritant than glycolic acid, since the pH value of synthetic prodrug was higher than that of glycolic acid. In the penetration test through nude mouse skin by diffusion cell, ethyl glycolate was continuously hydrolyzed to glycolic acid, which was assayed form the receptor compartment. It was obtained that the penetrated amount of ethyl glycolate was five times higher than that of glycolic acid. These results suggest that ethyl glycolate might be a successful prodrug of glycolic acid to reduce the skin irritation and to increase the skin penetration as well.

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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.