• Title/Summary/Keyword: aqueous methanol

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Kinetics and Mechanism of the Hydrolysis of Diazidophenylmethane Derivatives (Diazidophenylmethane 유도체들의 가수분해반응 메카니즘에 대한 반응속도론적 연구)

  • Kwon, Ki Sung;Seo, Jee Hyung;Lee, Yong Gu
    • Journal of the Korean Chemical Society
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    • v.41 no.6
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    • pp.313-319
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    • 1997
  • Diazidophenylmethane derivatives(X: p-H, $p-OCH_3,\;p-F,\;p-CH_3$) were synthesized and the rate constants of hydrolysis of diazidophenylmethane derivatives were determined by UV spectrophotometry in 50:50(v/v) aqueous methanol at 25$^{\circ}C$. On the basis of rate equation, substituent effect, activation parameters, solvent effect, salt effect, and product analysis, it may be concluded that the hydrolysis of diazidophenylmethane derivatives proceed through $S_N2_CA$ mechanism below pH 2.0, while above pH 12.0 through $S_N2$ mechanism, and in the range of pH from 2 to 12 through $S_N1$ mechanism respectively.

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Assessment of free-radical-scavenging and antibacterial activities, and brine shrimp toxicity of Scutellaria pinnatifida (Lamiaceae)

  • Sauvage, Severine;Samson, Emilie;Granger, Melanie;Majumdar, Anisha;Nigam, Poonam;Nahar, Lutfun;Celik, Sezgin;Sarker, Satyajit D.
    • Advances in Traditional Medicine
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    • v.10 no.4
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    • pp.304-309
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    • 2010
  • Scutellaria pinnatifida A. Hamilt. (Lamiaceae) is an endemic Turkish herb. This plant is also endemic to Iran, and grows abundantly in other central and western Asian countries. Several species of the Scutellaria are known for their traditional uses in the treatment of hypertension, arteriosclerosis, inflammatory diseases, hepatitis, allergy, cancer and diarrhoea. Free-radical-scavenging property, antibacterial activity and brine shrimp toxicity of the n-hexane, dichloromethane (DCM) and methanol (MeOH) extracts of S. pinnatifida were assessed using the 2,2-diphenyl-1-picryl-hydrazyl (DPPH) assay, the resazurin microtitre plate based assay, and the brine shrimp lethality assay, respectively. The DCM and MeOH extracts exhibited free-radical-scavenging property, with the $RC_{50}$ values of 0.362 and 0.127 mg/ml, respectively. Among the solid-phase extraction fractions of the MeOH extract, the 50% aqueous-MeOH fraction showed the highest level of free-radicalscavenging activity ($RC_{50}$ = 0.039 mg/ml). While the DCM extract showed low level of antibacterial activity against Bacillus subtilis and ampicillin-resistant Escherichia coli, the MeOH extract was active against B. cereus, B. subtilis, E. coli and ampicillin-resistant E. coli. However, the minimum inhibitory concentrations (MIC) of the MeOH extract against these bacterial strains were >10 mg/ml. None of the extracts showed any significant toxicity towards brine shrimps ($LD_{50}$ = > 1.00 mg/ml).

Extractives from Epimedium koreanum Nakai (삼지구엽초(Epimedium koreanum Nakai)의 추출성분)

  • Lee, Tae-Seong;Cho, Jae-Hyun;Hwang, Byung-Ho
    • Journal of Korea Foresty Energy
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    • v.24 no.2
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    • pp.16-23
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    • 2005
  • The air dried of Epimedium koreanum Nakai was extracted with MeOH and its extractives were concentrated with a vacuum evaporator. The extractives were fractionated with a series of n-hexane, chloroform (${CHCl}_3$), butanol (BuOH), ethyl acetate (EtOAc) and water on a separately funnel. Each fraction was freeze dried to give some dark brown powder. The EtOAc and BuOH soluble fractions were chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-n-hexane mixture as eluents. The isolated compounds were tested with a cellulose TLC developed with TBA and 6% acetic acid and then visualized on UV lamp or sprayed with vanillin-HCl-EtOH. The purified compounds were flavonoids and their glycosides, and organic acid as follows : (+)-catechin, icariin, hyperoside, Ikarisoside A and caffeic acid. The structures of each compounds were confirmed by $^1H-NMR,\;^{13}C-NMR$ and Mass spectra. Also, executed qualitative analysis as use GC/MS(Libraries search) about ${CHCl}_3$ soluble compounds of each part.

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Radical Scavenging Potential of Hydrophilic Phlorotannins of Hizikia fusiformis

  • Siriwardhana, Nalin;Lee, Ki-Wan;Jeon, You-Jin
    • ALGAE
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    • v.20 no.1
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    • pp.69-75
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    • 2005
  • Hizikia fusiformis is well known edible brown seaweed both in Korea and Japan. It has been intensively studied due to its pronounced health benefits. In this study, the radical scavenging (antioxidative) activities of its hydrophilic phlorotannin constituents were studied. An aqueous extract/original extract (OE) of H. fusiformis was initially prepared with heat, enzymes and pH control treatments. Then the original extract was further fractionated (with methylene chloride and methanol) and crude hydrophilic phlorotannin extract (CHPE) was prepared. The radical scavenging activities of both OE and CHPE were determined by using electron spin resonance (ESR) spectrophotometric assays such as 1,1-diphenyl-2-picrylhydrazyl (DPPH), hydroxyl and alkyl radical assays. The CHPE reported significantly (p < 0.05) higher total phenolic (phlorotannins) content (1.23 mg ${\cdot}ml^{-1}$) than that of the OE (0.21 mg ${\cdot}ml^{-1}$). Both OE and CHPE have reported good radical scavenging activities and those activities were dose-dependent. The CHPE have demonstrated significantly higher radical scavenging activities than that of the OE. In comparison, the DPPH radical (6 $\times$ 10$^{-5}$ M) scavenging activities of all the CHPE concentrations (0.25, 0.5 and 1 mg ${\cdot}ml^{-1}$) tested were significantly higher (37.3, 78.2 and 91.6%, respectively) than that of the OE counterparts (11.4, 34.6 and 61.7%, respectively). Alkyl radical scavenging percentages of CHPE at 0.0625, 0.125, 0.25 and 0.5 mg${\cdot}ml^{-1}$ were significantly higher (34.3, 69.2, 80.4 and 88.7%, respectively) than that of the OE (16.6, 41.4, 62.3 and 77.4%, respectively). The percentages of hydroxyl radical scavenging activities of CHPE at the concentrations of 0.25, 0.5 and 1 mg ${\cdot}ml^{-1}$ were 32.5, 59.4 and 84.2 % respectively. Moreover, the hydroxyl radical scavenging activity of OE was quite lower than that of the CHPE. Therefore, these results suggest that the hydrophilic phlorotannins of H. fusiformis are potential radical scavengers thus, a great source of antioxidative nutraceuticles.

Effects of Eucommiae Cortex on Osteoblast-like Cell Proliferation and Osteoclast Inhibition

  • Ha, Hyek-Yung;Ho, Jinn-Yung;Shin, Sun-Mi;Kim, Hye-Jin;Koo, Sung-Ja;Kim, In-Ho;Kim, Chung-Sook
    • Archives of Pharmacal Research
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    • v.26 no.11
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    • pp.929-936
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    • 2003
  • Methanol extract (MeOH), n-hexane (Hx), chloroform ($CHCl_3$), ethyl acetate (EA), butanol (BuOH) and aqueous ($H_2O$) fractions of Eucommiae Cortex including geniposidic acid (GA), geniposide (GP) and aucubin (AU) were tested for their therapeutic efficacy on osteoporosis. The contents of GA, GP and AU in the cortex and leaf of Eucommia ulmoides Oliver were quantified by HPLC. The effect of Eucommiae Cortex on the induction of growth hormone (GH) release was studied by using rat pituitary cells. The proliferation of osteoblast-like cells increased by herbal extracts was assayed using a tetrazolium (MTT), alkaline phosphatase (ALP) activity, and [$^3H$]-proline incorporation assays. The inhibition of osteoclast was studied by using the coculture of mouse bone marrow cells and ST-2 cells. As a result, the GA, GP and AU were present in the cortex more than in the leaf of E. ulmoides Oliver. The MeOH (1mg/mL), Hx, $CHCl_3$ and EA fractions (each 20 $\mu$ g/mL) had potent induction of GH release. The $CHCl_3$ exhibited the potent proliferation of osteoblasts. The AU, GP and GA were increased proliferation of osteoblasts. In addition, GA ($IC_{50}: 4.43{\times}10^{-7}$M), AU and GP were significantly inhibited proliferation of osteoclast. In summary, it is thought that the components in a part of the fractions of Eucommiae Cortex participate in each step of mechanism for activating osteoblast to facilitate osteogenesis, and suppress osteoclast activity to inhibit osteolysis.

Physicochemical Characterization and NMR Assignments of Ginsenosides Rb1, Rb2, Rc, and Rd Isolated from Panax ginseng

  • Cho, Jin-Gyeong;Lee, Min-Kyung;Lee, Jae-Woong;Park, Hee-Jung;Lee, Dae-Young;Lee, Youn-Hyung;Yang, Deok-Chun;Baek, Nam-In
    • Journal of Ginseng Research
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    • v.34 no.2
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    • pp.113-121
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    • 2010
  • The fresh ginseng roots were extracted with aqueous methanol, and the obtained extracts were partitioned using ethyl acetate, n-butanol, and water, successively. The repeated silica gel and octadecyl silica gel column chromatogaraphy for n-butanol fraction afforded four diol ginseng saponins, ginsenosides $Rb_1$, $Rb_2$, $R_c$, and Rd. The physicochemical, spectroscopic, and chromatographic characteristics of these ginsenosides were measured and compared with those reported in the literature. Some of the peak assignments in previously published $^1H$- and $^{13}C$-nuclear magnetic resonance (NMR) spectra were inaccurate. This study employed two-dimensional NMR experiments, including $^1H-^1H$ correlation spectroscopy, heteronuclear single quantum correlation, and heteronuclear multiple bond connectivity, to determine exact peak assignments.

Protein Kinase C Receptor Binding Assay for the Detection of Chemopreventive Agents from Natural Products

  • An, Geon-Ho;Suh, Young-Bae;Son, Kun-Ho;Chang, Il-Moo;Mar, Woong-Chon
    • Natural Product Sciences
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    • v.3 no.1
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    • pp.29-37
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    • 1997
  • Protein Kinase C (PKC) is generally believed to play a central role in signal transduction, cellular growth control, gene expression, and tumor promotion. And it has been suggested that inhibitors of PKC might play important roles for the prevention and treatment of cancer. In order to investigate the possible inhibitors of PKC from natural products, PKC receptor binding assay was performed using bovine brain particulate as a source of PKC and the amount of $[^3H]Phorbol$ 12,13-dibutyrate (PDBu) bound to PKC was measured in the presence of test materials. Total methanol extracts from 100 kinds of natural products were partitioned into 3 fractions (n-hexane, ethyl acetate and aqueous layer) and their binding ability to the regulatory domain of PKC was evaluated. The ethyl acetate fractions of Morus alba $(roots,\;IC_{50}:\;156.6\;{\mu}g/ml)$, Rehmannia glutinosa $(roots,\;IC_{50}:\;134.3\;{\mu}g/ml)$, Lysimachia foenum-graecum $(roots,\;IC_{50}:\;167.8\;{\mu}g/ml)$, Polygonum cuspidata $(roots,\;IC_{50}:\;157.3\;{\mu}g/ml)$, Cnidium officinale $(aerial\;parts,\;IC_{50}:\;145.2\;{\mu}g/ml)$, and the hexane $(IC_{50}:\;179.3\;{\mu}g/ml)$ and the EtOAc fraction of Symplocarpus nipponicus $(roots,\;IC_{50}:\;155.9\;{\mu}g/ml)$ showed inhibitory activity of $[^3H]PDBu$ binding to PKC.

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Applicability of Fibrous Solid Phase Extraction to Alkyl Phthalates Analysis (알킬프탈레이트 분석을 위한 섬유상 고상 추출법의 적용 가능성)

  • Jung, Yong-Jun
    • Journal of Korean Society on Water Environment
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    • v.24 no.6
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    • pp.801-805
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    • 2008
  • A fibrous material (p-phenylene-2,5-benzobisoxazole, PBO) was used as an adsorbent for solid phase extraction in order to simplify the extraction procedure. The extraction performance for di-(2-ethylhexyl) phthalate (DEHP) was examined with two types of PBO fibers (HM (High modulus) and AS (Regular type) types) by batch type sorption/desorption experiments. When 100 mg of the HM fibers were applied to 20 mL of the aqueous DEHP solution (less than $50{\mu}g/L$), more than 95% of DEHP was adsorbed on the fibers, however, the AS type fibers adsorbed alkyl phthalate up to 80%. In the case of $50{\mu}g/L$ of the initial concentration of DEHP, the adsorbed DEHP was extracted effectively with methanol and the maximum overall recovery ratio was 92.3%. The results indicated that the PBO fibers could be used as an adsorbent for alkyl phthalate analysis, and that the extraction procedure was not affected by suspended solids in a water sample.

Simultaneous Quantification of Oleins (triolein, diolein and monoolein) in Mouse Feces using Liquid Chromatography-Electrospray Ionization/Mass Spectrometry

  • Lim, Jong-Hyun;Lee, Jeong-Ae;Jang, Yu-Ra;Chung, He-Sson;Lee, Won-Yong;Chung, Bong-Chul
    • Mass Spectrometry Letters
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    • v.3 no.3
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    • pp.68-73
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    • 2012
  • Fat malabsorption is an important cause of poor growth in infancy and childhood. Steatorrhea tests have been developed using various methods. Traditional measurements of stool fat, however, require large samples and it often takes as a week to complete the analysis. In this paper, a liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI/MS) method was developed for simultaneous quantitative analysis of triacylglycerols, triolein, diolein and monoolein, in mouse feces. Moreover, the procedure was rapid, simple as well as compatible with LC-ESI/MS. Chloroform-isopropyl alcohol solution was used for fat-soluble sample extraction. After centrifugation and filtration, an analytical solution was prepared. Triolein, diolein and monoolein were separated using non-aqueous reversed-phase column with the mobile phase consisting of A (methanol) and B (acetone-isopropyl alcohol). The precision (% CV) and accuracy (% bias) of the assay were 3.8-14.7% and 85.2-114.9%, respectively. This method has been successfully applied to simultaneous determination of triolein, diolein and monoolein in feces from 30 mice. This method can therefore be applied to measure triacylglycerols in mouse feces accurately and precisely by LC-ESI/MS, thereby helping to predictive biomarker in fat malabsorption and diagnostic research.

Extractives from the leaves of Chamaecyparis obtusa Endlicher (편백나무(Chamaecyparis obtusa Endlicher) 잎의 추출성분)

  • Lee, Sang-Keug;Kim, Jin-Kyu;Ham, Yeon-Ho;Bae, Young-Soo
    • Journal of Forest and Environmental Science
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    • v.18 no.1
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    • pp.53-60
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    • 2001
  • 2kg of the dried leaves of chamaecyparis obtusa Endlicher were ground, extracted with acetone-$H_2O$(7:3, v/v), concentrated, and fractionated with a series of hexane, $CH_2Cl_2$, EtOAc and water on a separatory funnel. Each fraction was freeze dried to give dark-brown powder and a EtOAc soluble portion of the powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. Spectrometric analyses such as NMR and FAB-MS including TLC were performed to characterize the structures of the isolated compounds. The leaves of chamaecyparis obtusa Endlicher contained a large amount of taxifolin-3-O-${\beta}$-D-xylopyranoside and (+)-catechin in addition to a small amount of quercetin-3-O-${\alpha}$-L-rhamnopyranoside.

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