• Title/Summary/Keyword: NMR study

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Naltriben Analogues as Peptide Anticancer Drugs

  • Kim, Min-Woo;Shin, Choon-Shik;Yang, Hee-Jung;Kim, Seung-Hyun;Lim, Hae-Young;Lee, Chul-Hoon;Kim, Min-Kyun;Lim, Yoong-Ho
    • Journal of Microbiology and Biotechnology
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    • v.14 no.4
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    • pp.881-884
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    • 2004
  • Apoptosis inducers for cancer therapy have been studied. Among hundreds of inducers, peptide anticancer drugs have many advantages such as being not harmful to humans, high selectivity, and dependence on their structures. Naltriben (NTB) is an octapeptide consisting of DPhe-Cys-Tyr-DTrp-Orn-Thr-Pen-Thr-$NH_2$. Several NTB analogues are known. In this experiment, apoptotic activities of NTB analogues with 8 amino acids were tested using flow cytometry. The conformational study of NTB was carried out using NMR spectroscopy and molecular modeling. Here, the relationships between conformations of NTB analogues and their apoptotic effects are reported.

Synthesis and Characterization of 2, 6-Di-(4'-Methyl Phenyl) Pyrylium Fluoroborate and Perchlorate in Single Step Salts Using 4'-Methyl Acetophenone

  • Wie, Jin-Hyeong;Hong, Young-Min;Kim, Hyun-Ook;Kim, Kyung-Hoon;Cho, Sung-Il
    • Journal of Sensor Science and Technology
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    • v.21 no.1
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    • pp.13-20
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    • 2012
  • Due to its high conductivity, pyrylium has been frequently used in electron transfer reactions or in the synthesis of various organic materials. It has also been used as a sensor material. Traditionally, the compounds have been synthesized using various methods; mostly in a multiple steps. In this study, two pyrylium salts, 2, 6-di-(4'-methylphenyl) pyrylium fluoroborate and perchlorate were synthesized. The synthesis of these products was confirmed by 1H-NMR, LC/TOF-MS and FT-IR analyses while their photo-properties were analyzed using UV/VIS spectrophotometry. In addition, the electron transfer capacities of the salts were analyzed with a conductivity meter, it was found that their electron conductivities were high. When the synthesized compounds were dissolved in acetone, a green fluorescent material was observed to form. The fluorescent material can be used as a sensitizer in the electrical industry.

A Conformational Isomer of Soulattrolide from the Stem Bark of Calophyllum symingtonianum and Its Antibacterial Activity

  • Susanti, Deny;Attoumani, Nissad;Taher, Muhammad;Rezali, Mohd Fazlin;Sohrab, Md. Hossain;Hasan, Choudhury Mahmood;Zakaria, Zainul Amiruddin
    • Natural Product Sciences
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    • v.24 no.1
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    • pp.47-53
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    • 2018
  • Callophylum symingtonianum (Guttiferae), an evergreen broad-leaved tree that usually grows in hill forests, can be found distributed in the Malay Peninsula. The barks, leaves, flowers and seeds is often used medicinally to treat diarrhea and rheumatism. In the present study, we isolated two inophyllum type coumarins, 12-O-ethylinophyllum D (1) and iso-soulattrolide (2) from the stembarks of C. symingtonianum together with their antibacterial activity. The compounds were isolated by chromatographic methods on a silica gel. The structures were established by spectroscopic methods including UV, IR, (1D and 2D) NMR and mass spectrometry as well as by comparison with several literature sources. The antibacterial activity of those compounds was tested using a disc-diffusion assay against Staphylococcus aureus, Bacillus cereus, Escherichia coli and Pseudomonas aeruginosa. Both compound exhibited mild inhibition against P. aeruginosa with both $111{\mu}g/ml$ MIC value. Compound 2 also inhibits S. aureus with $25{\mu}g/ml$ MIC value.

Simultaneous Quantitative Analysis of Flavonoids Isolated from the Leaves of Diospyros kaki (감나무 잎으로부터 분리된 플라보노이드의 동시 정량분석)

  • Kim, Ga-Ram;Kim, Eun-Nam;Jeong, Gil-Saeng
    • Korean Journal of Pharmacognosy
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    • v.51 no.2
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    • pp.139-145
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    • 2020
  • The leaves of Diospyros kaki Thunb. were used to treat heart disease and hypotension in traditionally East Asia. The purpose of this study is to simultaneously quantitiative analyze the content of flavonoids in leaves of D. kaki. The isolated flavonoids from the leaves of D. kaki, and the structure of the isolated flavonoids were analyzed based on 1H and 13C NMR spectrum compared to literature data. Simultaneous quantitative analysis of the isolated flavonoids was validated using high performance liquid chromatography (HPLC). Results showed that the calibration curves of the flavonoid compounds were confirmed that they have a large linearity with a correlation coefficient (R2) of 0.99. In the intra-day and inter-day analysis, accuracy and precision of five compounds were measured that accuracy was 94.39 to 114.47% and precision was less than 3.00%. Content analysis showed hyperoside (1.30 ± 0.09%), astragalin (0.81 ± 0.06%), trifoline (1.58 ± 0.07%), quercetin (0.13 ± 0.02%) and kaempferol (1.33 ± 0.25%).

Isolation of Flavonoids from Processed Aconiti Tuber

  • Lyu, Ha-Na;Kwak, Ho-Young;Lee, Dae-Young;Kim, Kyong-Tai;Kim, Se-Young;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.51 no.4
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    • pp.165-168
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    • 2008
  • A processed Aconiti tuber (Korean name, Kyeong-Po Buja) was extracted with 80% aqueous EtOH, and the concentrated extract was partitioned with EtOAc and water ($H_2O$). From the EtOAc fraction, two flavonoids were isolated through repeated silica gel column chromatographies. From the result of physico-chemical data including NMR, mass spectrometry and IR, the chemical structures of the compounds were determined to be liquiritin (1) and liquiritigenin (2). This is the first study to isolate flavonoids (1) and (2) from the processed Aconiti tuber.

Extraction and Bioassay of Allelochemicals in Jerusalem Artichoke

  • Sungwook Chae;Lee, Ho-Jin
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.46 no.4
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    • pp.309-316
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    • 2001
  • Helianthus tuberosus has been known to inhibit the growth of weeds and other plants sharing its habitat. This study was conducted to identify the allelochemicals of Helianthus tuberosus which were extracted with water and solvents. Aqueous extracts of leaf, stem, root, tuber and tuber peel of Helianthus tuberosus except tuber did not show significant differences in phytotoxicity to alfalfa seedlings. It was considered that Helianthus tuberosus contained fewer or less potential water-soluble substances that were toxic to alfalfa. Methanol extract of leaves of Helianthus tuberosus was sequentially partitioned in increasing polarity with n-hexane, ethylacetate and n-butanol. Each extract had a yield of 148, 12, 15.7 and 9.5g, respectively. Inhibitory effects on germination of alfalfa seeds treated with four fractions were not significantly different. But the significant reductions on hypocotyl length were observed for all the solvent extracts. Among the four fractions, the ethylacetate fraction showed the most significant inhibition effect on bioassay with alfalfa. Further separation of the active ethylacetate fraction by open column chromatography led to the 25 subfractions. In bioassay of each sub-fraction with alfalfa seeds, sub-fraction No. 13 showed the most inhibitory effect on seedling growth. $^1$H NMR and gas chromatography-mass spectrometry analysis revealed that sub-fraction No. 13 was the mixture of straight-chain saturated fatty acids.

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Synthesis and Application for Hydrophilic Polyurethane of Non-swelling Type (Non-swelling type의 Hydrophilic polyurethane 합성 및 응용에 관한 연구)

  • Yang, Jeong-Han;Jeon, Jae-Woo;Yeum, Jeong-Hyun;Kim, Duck-Han;Oh, Kyoung-Suk;Yoon, Nam-Sik
    • Textile Coloration and Finishing
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    • v.23 no.2
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    • pp.118-130
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    • 2011
  • In this study, hydrophilic polyurethane (PU) was synthesized by one shot process to get good non-swelling effect and to keep high breathability using reactive silicone oil of mono terminal and bi-terminal types. We also blended non reactive silicone oil with pure hydrophilic PU to compare non-swelling effect and breathability with hydrophilic PU synthesized by the two types of reactive silicone oils. The hydrophilic films were analyzed by nuclear magnetic resonance (NMR) spectroscopy, scanning electron microscope (SEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray photo electron (XPS) spectroscopy, energy dispersive spectrometry (EDS), breathability, waterproofness, tensile strength, contact angle and swelling effect. The results showed that the film made by hydrophilic PU which was synthesized with mono terminal type silicone oil provided good non-swelling effect and acceptable moisture permeability due to the modified surface properties.

A study on the structural and electric properties of fluorinated $YBa_2Cu_3O_{7-y}$ (불소화된 $YBa_2Cu_3O_{7-y}$ 초전도체의 구조적, 전기적 성질에 관한 연구)

  • 김재욱;김채옥
    • Electrical & Electronic Materials
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    • v.9 no.4
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    • pp.404-409
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    • 1996
  • The structural and electric properties of $Y_{1-x}$YbF$_{x}$Ba$_{2}$Cu$_{3}$O$_{7-y}$(x=0.0, 0.1, 0.2, 0.3, 0.4, 0.5 and 0.6) have been investigated by using XRD(X-ray diffraction), TMA(thennomechanical analysis), NMR(nuclear magnetic resonance) analysis and four probe method. $Y_{1-x}$YbF$_{x}$Ba$_{2}$Cu$_{3}$O$_{7-y}$ samples were prepared by conventional solid-state reaction method using $Y_{2}$O$_{3}$, BaCO$_{3}$, CuO and YbF$_{3}$ power. TMA and high temperature XRD results shows that orthorhombic to tetragonal phase transition occurs in the unfluorinated 1-2-3 sample while the phase change is not observed in the fluorinated 1-2-3 samples. Superconducting transition temperature(T$_{c}$) increases with increasing YbF$_{3}$ content ; T$_{c}$, of the sample reaching maximum of 102K for x=0.3, and then decreases with further increasing YbF$_{3}$ content. The structural analysis and T$_{c}$ results shows that the fluorine doping stabilize the orthorhombic phase, together with the increase in T$_{c}$.}$ c/.TEX> c/.

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Carbon-13 and Vanadium-51 Nuclear Magnetic Resonance Studies of Vanadium(v)-Aminopolycarboxylic Acids (Ⅰ) (바나듐 (v)-아미노폴리카르본산 착물의 탄소-13 및 바나듐-51 핵자기공명연구 (제1보))

  • Man-Ho Lee;Tae-Sub O
    • Journal of the Korean Chemical Society
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    • v.27 no.2
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    • pp.117-126
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    • 1983
  • $^13C$ and $^51V$ NMR spectroscopy have been used to study the solution structures of the vanadium (v) complexes formed by ethylenediaminetetraacetic acid (EDTA), trans-cyclohexanediaminetetraacetic acid (CDTA), 1,2-propylenediaminetetraacetic acid (PDTA), ethylenediaminediacetic acid (EDDA), 2-hydroxyethylethylenediaminetriacetic acid (HEDTA), diethylenetriaminepentacetic acid (DPTA), and nitrilotriacetic acid (NTA). All of the complexes probably have octahedral structures containiing cis-$VO_2$ core. The coordination of hydroxylethyl group is found to be less favored than that of acetate group. EDDA forms two isomers, ${\alpha}$-cis and ${\beta}$-cis. PDTA also forms two structural isomers due to the methyl group in the ligand.

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Synthesis of UV-Curable Modified (3,4-epoxycyclohexane)methyl 3,4-epoxycyclohexylcarboxylate Acrylate (자외선 경화형 변성 (3,4-epoxycyclohexane)methyl 3,4-epoxycyclohexylcarboxylate 아크릴레이트의 합성)

  • Lee, Jongmin;Yi, Hwanpyo;Lee, Sanggun;Park, Hyungnam;Choi, Kangsik;Kim, Dojin
    • Korean Journal of Materials Research
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    • v.27 no.4
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    • pp.199-205
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    • 2017
  • In this study, (3,4-epoxycyclohexane)methyl 3,4-epoxycyclohexylcarboxylate acrylate was synthesized by reacting (3,4-epoxycyclohexane)methyl 3,4-epoxycyclohexylcarboxylate with acrylic acid to minimize hardening shrinkage and to improve heat resistance, which are known as disadvantages of photopolymers for 3D printing application. Urethane acrylate was synthesized by reacting 1,3,5-triazine-2,4,6-triamino alcohol, 2-hexylethyl acrylate, and isophorone diisocyanate in order to improve the mechanical properties without deteriorating the heat resistance. The physical properties before and after the synthesis of the acrylate and the mechanical properties when the urethane acrylate was applied were investigated. The reaction progress of the composite was examined by FTIR and $^{13}C$ NMR. The heat deflection temperature, flexural strength, and surface hardness of the molding were measured. The curing behavior by Photo-DSC ultraviolet irradiation was also examined.