• Title/Summary/Keyword: $^{13}C$ NMR spectrum

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Study of CO2 Absorption Characteristic and Synthesis of 1-(2-methoxyethyl)-3-methylimidazoLium Methanesulfonate Ionic Liquid (1-(2-methoxyethyl)-3-methylimidazolium Methanesulfonate 이온성 액체 합성 및 CO2 흡수 특성 연구)

  • Jin, Yu Ran;Jung, Yoon Ho;Park, So Jin;Baek, Il Hyun
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.35-40
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    • 2012
  • In this study, 1-(2-methoxyethyl)-3-methylimidazolium methanesulfonate ionic liquid has been synthesized, characterized and tested with respect to carbon dioxide absorption with the aim to use it as advanced absorbent materials in fossil fuel processing. The ionic liquid was synthesized by a one step method, low cost. The thermal and chemical stability of selected ionic liquid has been investigated by DSC, TGA and the structure was verified by $^1H$-NMR spectroscopy. The solubility of carbon dioxide in the methanesulfonate-based ionic liquids were measured using a high-pressure equilibrium apparatus equipped with a variable-volume view cell at 30, 50 and $70^{\circ}C$ and pressure up to 195 bar. The results show that carbon dioxide solubilities of 1-(2-methoxyethyl)-3-methylimidazolium methanesulfonate increased with pressure increasing and temperature decreasing, and the carbon dioxide absorption capacity showed 27.6 $CO_2/IL$(g/kg) at $30^{\circ}C$, 13 bar.

Inductive Effects of the Cold Receptor TRPM8 Expression in Ganoderma lucidum Extracts and Ergosterol (영지버섯추출물 및 에르고스테롤의 냉감 수용체 TRPM8 (Transient Receptor Potential Cation Channel Melastatin Subtype 8) 발현 유도 효과)

  • Ryu, Hwa Sun;Jeong, JiYeon;Jeon, Weon-Ok;Lee, Chun Mong;Lee, Jung-No;Park, Sung-Min
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.44 no.1
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    • pp.15-21
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    • 2018
  • Skin-aging is accelerated by the increased expression of MMP-1 caused by the increased skin temperature induced by IR/visible light as well as UV. Thus, the control of skin temperature is important to inhibit heat-induced aging. Many studies have been conducted to lower the skin temperature through the controlling transient receptor potential melastatin 8 channel (TRPM8), which is known as the cold and menthol receptor 1 (CMR1) and is activated at temperature below $25^{\circ}C$. In this study, we first investigated the effect of Ganoderma lucidum extract (GLE) on the TRPM8 expression. Results showed that GLE, hexane (Hex) fractions and water fractions increased the TRPM8 expression in a dose dependent manner. Active compound in Hex fractions were separated by chromatography and analyzed by $^1H$ and $^{13}C$ NMR spectroscopy. The isolated compounds were identified as ergosterol and it also significantly increased the TRPM8 expression. Taken together, these results strongly suggest that G. lucidum extract and ergosterol have the potential as a new cooling ingredient in the cosmetics.

Identification of Maysin and Related Flavonid Analogues in Corn Silks (옥수수 수염에서 Maysin 및 유사물질의 동정)

  • Kim, Sun-Lim;Snook, Maurice E.;Kim, E-Hun;Park, Cheol-Ho
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.45 no.3
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    • pp.151-157
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    • 2000
  • This study was carried out to isolate and identify the maysin and related flavonoid analogues in corn silks. Silks were covered with silk bag to prevent pollination and were sampled at 3-5 days after silking. The silks were filled with 100% MeOH and stored at $0^{\circ}C$ until analysis. The MeOH extracts of corn silks were filtered and concentrated at 35-4$0^{\circ}C$. The ${CH}_2$${Cl}_2$ was added on the concentrated aqueous solution to remove the chlorophyll and lipids. The Cis open column (25mm$\times$54 cm) was washed and activated with serial treatment of 500$m\ell$ of 100% MeOH(twice)longrightarrow75% MeOH longrightarrow50% MeOHlongrightarrow30% MeOHlongrightarrow100% $H_2$O(2 times). The concentrated aqueous solution was applied to the $C_{18}$ column and washed with $H_2O$ several times to remove the sugars and water soluble pigments. Neochlorogenic acid, chlorogenic acid and 4-caffeoylquinic acid were eluted with 10% MeOH, and rhamosyl isoorientin was eluted with 30% MeOH, but maysin was eluted with 50% MeOH from the $C_18$ open column. Collected fractions were analyzed with HPLC by using revers-phase Ultras-phere $C_{18}$ column (4.6$\times$250mm, 5$\mu\textrm{m}$) and $H_2$O (10% MeOH containing 0.1% $H_3$${PO}_4$)/MeOH (100% MeOH containing 0.1% H$_3$PO$_4$) linear gradient from 20% to 90% MeOH for 35 minutes, a flow rate of 1 $m\ell$/min and detection at 340nm. The selected fractions were concentrated and applied to the silicic acid column. Maysin was eluted with 500$m\ell$ of 100% ethyl acetate from the silicic acid column for the first purification, and the purity of collected fractions was about 75%, but the purity from the second purification with the Cis column (1/2 $\times$ 43") was greater than 95%. FAB-MS spectral data was obtained with VG7O-VSEQ VG analytical fast atom bombardment mass (UK). $^1$H-NMR and $^{13}$ C-NMR data were obtained with Bruker DPX 400 MHz NMR spectrometers (German) in DMSO-d$_{6}$ at 400 and 100 MHz, respectively.vely.

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Synthesis and Spectroscopic Characterization of Manganese(II), Iron(III) and Cobalt(III) Complexes of Macrocyclic Ligand. Potential of Cobalt(III) Complex in Biological Activity

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.
    • Journal of the Korean Chemical Society
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    • v.55 no.6
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    • pp.919-925
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    • 2011
  • A new series of manganese(II), iron(III) and cobalt(III) complexes of 14-membered macrocyclic ligand, (3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane-1,8-diamine) have been prepared and characterized by elemental analyses, IR, UV-VIS, $^1H$- and $^{13}C$- NMR spectra, magnetic susceptibilities, conductivities, and ESR measurements. Molar conductance measurements in DMF solution indicate that the complexes are electrolytes. The ESR spectrum for cobalt(III) complex in $CD_3OD+10%D_2O$ after exposure to $^{60}Co-{\gamma}$-rays at 77 K using a 0.2217 M rad $h^{-1}$ vicrad source showed $g_{\perp}$ > $g_{\parallel}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_z2$ orbital with covalent bond character. In this case, the ligand hyperfine tensors are nearly collinear with ${\gamma}$-tensors, so there is no major tendency to bend. Therefore, little extra delocalization via the ring lobe of the $dz^2$ orbital occurs. However, the ESR spectrum in solid state after exposure to $^{60}Co-{\gamma}$-rays at 77 K showed $g_{\parallel}$ > $g_{\perp}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_x2_{-y}2$ ground state as the resulting spectrum contains a large number of randomly oriented molecules provided that, the principle directions of g and A tensors. Manganese (II) complex 2, $[H_{12}LMn]Cl_4.2H_2O$, showed six isotropic lines characteristic to an unpaired electron interacting with a nucleus of spin 5/2, however, iron(III) complex 3, $[H_{12}LFe]Cl_5.H_2O$, showed spectrum of a high spin $^{57}Fe$ (I=1/2), $d^5$ configuration. The geometry of these complexes was supported by elemental analyses, IR, electronic and ESR spectral studies. Complex 1 showed exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Solution Processable Symmetric 4-Alkylethynylbenzene End-Capped Anthracene Derivatives

  • Jang, Sang-Hun;Kim, Hyun-Jin;Hwang, Min-Ji;Jeong, Eun-Bin;Yun, Hui-Jun;Lee, Dong-Hoon;Kim, Yun-Hi;Park, Chan-Eon;Yoon, Yong-Jin;Kwon, Soon-Ki;Lee, Sang-Gyeong
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.541-548
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    • 2012
  • New candidates composed of anthracene and 4-alkylethynylbenzene end-capped oligomers for OTFTs were synthesized under Sonogashira coupling reaction conditions. All oligomers were characterized by FT-IR, mass, UV-visible, and PL emission spectrum analyses, cyclic voltammetry (CV), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), $^1H$-NMR, and $^{13}C$-NMR. Investigation of their physical properties showed that the oligomers had high oxidation potential and thermal stability. Thin films of DHPEAnt and DDPEAnt were characterized by spin coating them onto Si/$SiO_2$ to fabricate top-contact OTFTs. The devices prepared using DHPEAnt and DDPEAnt showed hole field-effect mobilities of $4.0{\times}10^{-3}cm^2$/Vs and $2.0{\times}10^{-3}cm^2$/Vs, respectively, for solution-processed OTFTs.

A Highly Selective Staurosporine Derivative Designed by a New Selectivity Filter

  • El-Deeb, Ibrahim M.;Jung, Su-Jin;Park, Byung-Sun;Yoo, Young-Jun;Choi, Ki-Hang;Yang, Young-Mok;Lee, Sang-Woo;Kim, In-Tae;Han, Dong-Keun;Lee, So-Ha
    • Bulletin of the Korean Chemical Society
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    • v.32 no.5
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    • pp.1709-1714
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    • 2011
  • KIST301135 was semi-synthetically prepared by the reaction of Staurosporine with triphosgene in anhydrous dichloromethane. The structure of KIST301135 was confirmed by $^1H$ NMR, $^{13}C$ NMR, and high resolution mass spectrum. KIST301135 was initially tested in a single dose duplicate mode at a concentration of 20 nM over a panel of 53 kinases against Staurosporine as a positive control. KIST301135 has showed inhibitions above 75% in only 2 kinases (FLT3 and JAK3 kinases) of the 53 tested kinases, while Staurosporine has showed inhibitions above 80% in about 62% of the tested kinases. KIST301135 was retested at a 5-dose testing mode over the 9 kinases inhibited by percentages over 20 at the single dose testing in order to determine its $IC_{50}$ values. KIST301135 has shown much improved kinase inhibitory selectivity relative to Staurosporine in its potency at JAK3 kinase and CAMK2b kinase.

Characteristics of Cosmetic with Whitening Compounds from Phellodendron amurense (Phellodendron amurense의 미백물질을 이용한 화장품 특성)

  • Cho, Young-Je
    • Journal of Applied Biological Chemistry
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    • v.54 no.2
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    • pp.108-113
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    • 2011
  • The tyrosinase inhibitory activity of extracts from Phellodendron amurense was examined. Tyrosinase inhibitory activity of 60% ethanol extracts was determined as 25% and the inhibitory activity of 60% ethanol extracts against melanin biosynthesis in melanoma cell (B16F10) was 31.2%. The purified inhibitory compounds against tyrosinase by Sephadex LH-20, MCI-gel CHP-20 column chromatography from P. amurense was confirmed as obacunone by $^1H$-NMR, $^{13}C$-NMR and Fast atom bombardment (FAB)-Mass spectrum. The tyrosinase inhibitory activities of purified obacunone was respectively as 35.1%. The safety of essence with tyrosinase inhibitory compounds from P. amurense was also assayed by various safety profiles. First, pH and viscosity change of essence for 60 days were not detected. The essence also showed the stability against temperature and light for 60 days. All these findings suggest that extracts from P. amurense has a great potential as a cosmeceutical ingredient, which has a potent whitening effect.

Purification and Identification of Phenol Compounds with Inhibitory Activity on Helicobacter pylori from Rhododendron mucronulatum Flos. Extracts (진달래꽃(Rhododendron mucronulatum Flos.) 추출물로부터 Helicobacter pylori 억제 효과를 가지는 phenol성 물질의 정제 및 동정)

  • Ju, In-Sik;Cho, Young-Je
    • Journal of Life Science
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    • v.19 no.8
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    • pp.1125-1131
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    • 2009
  • The antimicrobial activities of Helicobacter pylori as a functional food source with water and 60% ethanol extracts from Rododendron mucronulatum Turcz. flowers were examined. The total phenol content of 60% ethanol extracts (30.6${\pm}$0.14 mg/g) from Rododendron mucronulatum Turcz. flowers was higher than that of water extracts (23.2${\pm}$0.21 mg/g). The inhibitory activities of Rododendron mucronulatum Turcz. extracts on H. pylori was determined to clear zone of 15 mm in 80% ethanol extracts. Purification of inhibitory compounds was carried out in Sephadex LH-20 and MCI-gel CHP-20 column chromatography using a gradient procedure, with increasing ethanol(0${\rightarrow}$100%) in $H_2O$. The chemical structure of the purified inhibitory compounds of H. pylori was identified to be quercitrin (quercetin-3-O- rhamnopyranoside), myricitrin (myricetin-3-O-rhamnopyranoside), quercetin by FAB-MS, NMR and IR spectra.

Synthesis and Physical Properties of Decylbithiophene End-Capped Oligomers Based on Naphthalene, Anthracene and Benzo[1,2-b:4,5-b']dithiophene

  • Jang, Sang-Hun;Tai, Truong Ba;Kim, Min-Kyu;Han, Jeong-Woo;Kim, Yun-Hi;Shin, Sung-Chul;Yoon, Yong-Jin;Kwon, Soon-Ki;Lee, Sang-Gyeong
    • Bulletin of the Korean Chemical Society
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    • v.30 no.3
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    • pp.618-622
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    • 2009
  • The new candidates for OTFTs, which were composed of naphthalene, anthracene, benzo[1,2-b:4,5-b’]dithiophene and 2-decylbithiophene end-capper were synthesized under Suzuki coupling reaction conditions. All of the oligomers were characterized by FT-IR, mass analysis, UV-vis, PL spectrum, cyclic voltametry (CV), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), $^1H-NMR\;and\;^{13}C-NMR$. Investigation of physical properties showed that all of the oligomers have higher oxidation potential and good thermal stability. Especially, DBT-DtB-DBT is soluble in common solvents and suitable for low cost processing technologies.

Modulative Effect of Human Hair Dermal Papilla Cell Apoptosis by Acertannin from the Barks and Xylems of Acer ginnala Maxim (신나무 유래 Acertannin의 인체 모유두 세포 Apoptosis 조절 효능)

  • Joung, Seo Woo;Choi, Sun Eun
    • Korean Journal of Pharmacognosy
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    • v.49 no.1
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    • pp.7-14
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    • 2018
  • We isolated gallotannin, 2,6-digalloyl-1,5-anhydroglucitol, known as acertannin (1), from the barks and xylems of Acer ginnala Maxim. It is a genus of Acer species of shrubs in the family Aceraceae. A. ginnala grows in Korea, Japan and Mongolia. We accomplished the structure elucidation by confirming that the result of $^1H$,$^{13}C-NMR$,MS spectrum data was similar to previous references. We measured DPPH and ABTS radical scavenging activity in vitro to evaluate anti-oxidative activities on acertannin isolated from A. ginnala. Acertannin from A. ginnala exhibited potent DPPH and ABTS radical scavenging activities. We examined the antioxidant and apoptosis modulative effects. This examination shows that A. ginnala has not only 1,1-diphenyl-2-picryhydrazyl(DPPH) radical scavenging activity and ABTS radical scavenging activity, but also human hair dermal papilla cell protection effects. These results indicate that the barks and xylems of A. ginnala might be developed as a potent anti-oxidant, hair growth agent, and ingredient for related new functional cosmetic materials.