• Title/Summary/Keyword: $^{13}C$ CP-Mass NMR

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Isolation and Purification of Berberine in Cortex Phellodendri by Centrifugal Partition Chromatography (Centrifugal Partition Chromatography에 의한 황백으로부터 Berberine의 분리 및 정제)

  • Kim, Jung-Bae;Bang, Byung-Ho
    • The Korean Journal of Food And Nutrition
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    • v.27 no.3
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    • pp.532-537
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    • 2014
  • Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections, and infections of the body surface. Many analytical methods have been used to study oriental herbal medicines, such as thin-layer chromatography, column liquid chromatography, and high performance liquid chromatography (HPLC). In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out in order to separate pure compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 mL/min in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. The $^1H$ NMR spectrum revealed that the resonances at ${\delta}$ 4.10 and 4.20 ppm corresponded to three protons ($-OCH_3$), whereas those at ${\delta}$ 6.10 ppm corresponded to two protons ($-OCH_2O-$). Further, two aromatic protons (H-11 and H-12) conveys a doublet-doublet pattern. The H-11 doublet and H-12 doublet appear at ${\delta}$ 7.98 and 8.11, respectively. The $^{13}C$ NMR. spectrum showed a tetrasubstituted with a methylenedioxy group at C2 and C3, and two methoxy groups at C9 and C10. The chemical structure of the berberine was identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

Chemical Characteristics of Cell Wall in Pinus thunbergii Parl. Grown with High Salinity (고염분 하에서 성장한 해송 세포벽의 화학 성상)

  • Kim, Kang-Jae;Eom, Tae-Jin
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.47 no.4
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    • pp.144-150
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    • 2015
  • Stems of Pinus thunbergii Parl. grown with high salinity were analyzed for chemical characteristics. Stem of 2 years was rich in soluble compounds and stem of 3 years reduced the amount of the soluble compound. But, the lignin content have not seen a large change. Also, Klason lignins of stem of 2 and 3 years has not changed in nitrogen and hydrogen content. In Klason process, it was significantly increased the carbon concentration due to the hydrolysis of the carbohydrate. In addition, the accumulation of xylan from Pinus thunbergii Parl. with salinity treatment were increased noticeably. Finally, functional group of Pinus thunbergii Parl. with salinity treatment were not changed.

Isolation and Purification of Antibacterial Components in Cortex Phellodendri (황백나무로부터 항균성분의 분리 및 정제)

  • Kim, Jung-Bae;Shin, Woon-Seob;Kwon, Young-In;Bang, Byung-Ho
    • The Korean Journal of Food And Nutrition
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    • v.26 no.3
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    • pp.547-552
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    • 2013
  • Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections and infections of the body surface. In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out to separate antibacterial compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 $m{\ell}/min$ in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. Palmatine weas identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

Preparation of Polymethylene-bridged Half-Titanocenes and Investigation of Their Styrene Polymerization Properties (폴리메틸렌 다리를 가진 Dinuclear Half-Titanocene 합성과 이에 의한 스티렌 중합 연구)

  • 태원태;김상현;노석균;김태학;이동호
    • Polymer(Korea)
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    • v.24 no.2
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    • pp.159-167
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    • 2000
  • The polymethylene-bridged dinuclear half-titanocenes [(CH$_2$)$_{n}$(C$_{5}$ H$_4$)$_2$][TiCl$_3$]$_2$ (n=5(10), 7(11), 9(12)) have been synthesized by treating the distannylated derivatives of the ligands with two equivalents of TiCl$_4$ in toluene. All complexes are characterized by IR, $^1$H NMR, $^{13}$ C NMR and mass spectrometry. In order to examine the catalytic properties of the dinuclear complexes styrene polymerization has been conducted in the presence of MMAO. From the polymerization experiments it was found that ( i ) all the prepared complexes 10-12 produced syndiotactic polystyrenes, ( ii ) the complex 12 holding the longest bridging ligand exhibited the highest activity but produced a polymer having the smallest molecular weight among the polymethylene-bridged dinuclear half-titanocenes. This behavior was attributed to the influence of electron-donating caused by the polymethylene bridge between two active centers as well as the effect of steric congestion around metal center caused by the proximal distance between two active sites.s.

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Chemical Characteristics of Abiotic-Stressed Tobacco Stems for the Utilization of a Non-Wooden Biomass (비목질 재료의 바이오매스화를 위한 환경 스트레스 담배줄기의 화학조성)

  • Kim, Kang-Jae;Hong, Sung-Bum;Eom, Tae-Jin
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.48 no.1
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    • pp.53-60
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    • 2016
  • Abiotic-stressed tobacco stems as a non-wooden biomass were analyzed for their chemical characteristics. Light-stressed tobacco stems (LST) have a relatively high nitrogen concentration, much more extractive content, and a similar amount of lignin and higher contents of acid sugars than those of Non stressed tobacco (NST). It also has low cellulose crystallinity and a high degree of condensation. Guaiacyl units having a lower molecular weight distribution consist of rich lignin. Tension stressed tobacco (TST) growth differentiation under tensile stress was significantly different between normal tissue and cell walls, with the exception of the slightly higher cellulose crystallinity observed for.