• Title/Summary/Keyword: solvent system

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Rapid Isolation of Cyanidin 3-Glucoside and Peonidin 3-Glucoside from Black Rice (Oryza sativa) Using High-Performance Countercurrent Chromatography and Reversed-Phase Column Chromatography

  • Jeon, Heejin;Choi, Janggyoo;Choi, Soo-Jung;Lee, Chang Uk;Yoon, Shin Hee;Kim, Jinwoong;Yoon, Kee Dong
    • Natural Product Sciences
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    • v.21 no.1
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    • pp.30-33
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    • 2015
  • Anthocyanins are water soluble plant pigments which are responsible for the blue, red, pink, violet colors in several plant organs such as flowers, fruits, leaves and roots. In recent years, anthocyanin-rich foods have been favored as dietary supplements and health care products due to diverse biological activities of anthocyanins including antioxidant, anti-allergic, anti-diabetic, anti-microbial, anti-cancer and preventing cardiovascular disease. High-performance countercurrent chromatography (HPCCC) coupled with reversed-phase medium pressure liquid chromatography (RP MPLC) method was applied for the rapid and efficient isolation of cyanidin 3-glucoside (C3G) and peonidin 3-glucoside (P3G) from black rice (Oryza sativa L., Poaceae). The crude black rice extract (500 mg) was subjected to HPCCC using two-phase solvent system composed of tert-butyl methyl ether/n-butanol/ acetonitrile/0.01% trifluoroacetic acid (TBME/B/A/0.01% TFA, 1 : 3 : 1 : 5, v/v, flow rate - 4.5 mL/min, reversed phase mode) to give enriched anthocyanin extract (37.4 mg), and enriched anthocyanin extract was sequentially chromatographed on RP-MPLC to yield C3G (16.5 mg) and P3G (8.7 mg). The recovery rate and purity of isolated C3G were 76.0% and 98.2%, respectively, and those of P3G were 58.3% and 96.3%, respectively. The present study indicates that HPCCC coupled with RP-MPLC method is more rapid and efficient than multi-step conventional column chromatography for the separation of anthocyanins.

The study of characterization of extracted vanadium in waste catalyst for vanadium redox flow battery (폐촉매에서 추출한 바나듐 레독스 흐름전지용 바나듐의 특성 연구)

  • Kang, Ung Il
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.10
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    • pp.598-602
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    • 2018
  • This study examined the characteristics of the waste catalyst used in the petroleum refinery operations. The total pore volume, specific surface area, and average pore size of the spent catalyst used in the petroleum refinery operations were 3.96cc/g, 13.81m2/g, and 1.15A, respectively. The weight loss observed in the range from $25^{\circ}C-700^{\circ}C$ for the spent catalysts using TG and DTA was approximately 23 wt. %. EDS analysis of the waste catalyst sample showed that the five major components were vanadium, nickel, manganese, iron, and copper. The extraction system is attractive for liquid-liquid extraction. In this study, Cynex 272 was used to extract vanadium from waste catalyst. The electrochemical characteristics of the extracted vanadium solution were measured by cyclic voltammetry (CV). As a result, an oxidation / reduction peak appeared, indicating the potential of an electrolytic solution.

An Antifungal Antibiotic Purified from Bacillus megaterium KL39, a Biocontrol Agent of Red-Pepper Phytophthora-Blight Disease

  • JUNG HEE KYOUNG;KIM SANG-DAL
    • Journal of Microbiology and Biotechnology
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    • v.15 no.5
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    • pp.1001-1010
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    • 2005
  • Bacillus megaterium KL39, an antibiotic-producing plant growth promoting rhizobacterium (PGPR), was selected from soil. The antifungal antibiotic, denoted KL39, was purified from culture filtrate by column chromatography using Dion HP-20, Silica gel, Sephadex LH-20, and prep-HPLC. Thin layer chromatography, employing the solvent system of ethanol:ammonia:water=8:1:1, showed the $R_{f}$. value of 0.32. The antibiotic KL39 showed a negative reaction with ninhydrin solution, positive with iodine vapor, and also positive with Ehrlich reagent. It was soluble in methanol, ethanol, butanol, and acetonitrile, but insoluble in chloroform, toluene, hexane, ethyl ether, or acetone. Its UV spectrum had the maximum absorption at 208 nm. Amino acid composition, FAB-mass, $^{1}H-NMR,\;^{13}C-NMR$, and atomic analyses showed that the antibiotic KL39 (MW=1,071) has a structure very similar to iturin E. The antibiotic KL39 has a broad antifungal spectrum against a variety of plant pathogenic fungi including Rhizoctonia solani, Pyricularia oryzae, Monilinia froeticola, Botrytis cinenea, Altenaria kikuchiana, Fusarium oxysporum, and F. solani. An MIC value of $10\;{\mu}g/ml$ was determined for Phytophthora capsici. Macromolecular incorporation studies with P. capsici using radioactive [$^{3}H-adenine$] as the precursor, indicated that the antibiotic KL39 strongly inhibits the DNA biosynthesis of the fungal cell. Microscopic observation of the antifungal action showed abnormal hyphal swelling of P. capsici. The purified antibiotic KL39 was very effective for the biocontrol of in vivo Phytophthora-blight disease of pepper.

Effect of spinning parameters of polyethersulfone based hollow fiber membranes on morphological and mechanical properties

  • Tewfik, Shadia R.;Sorour, Mohamed H.;Shaalan, Hayam F.;Hani, Heba A.
    • Membrane and Water Treatment
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    • v.9 no.1
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    • pp.43-51
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    • 2018
  • Hollow fiber (HF) membranes are gaining wide interest over flat membranes due to their compaction and high area to surface volume ratio. This work addresses the fabrication of HF from polysulfone (PS) and polyethersulfone (PES) using N-methylpyrrolidone (NMP) as solvent in addition to other additives to achieve desired characteristics. The semi-pilot spinning system includes jacketed vessel, four spinneret block, coagulation and washing baths in addition to dryer and winder. Different parameters affecting dry-wet spinning phase inversion process were investigated. Dope compositions of PES, NMP and polyvinyl pyrrolidone (PVP) of varying molecular weights as additive were addressed. Some critical parameters of importance were also investigated. Those include dope flow rate, air gap, coagulation & washing baths and drying temperatures. The measured dope viscosity was in the range from 1.7 to 36.5 Pa.s. Air gap distance was adjusted from 20 to 45 cm and coagulation bath temperature from 20 to $46^{\circ}C$. The HF membranes were characterized by scanning electron microscope (SEM), atomic force microscope (AFM) and mechanical properties. Results indicated prevalence of finger like structure and average surface roughness from about 29 to 78.3 nm. Profile of stress strain characteristics revealed suitability of the fibers for downstream interventions for fabrication of thin film composite membrane. Different empirical correlations were formulated which enable deeper understanding of the interaction of the above mentioned variables. Data of pure water permeability (PWP) confirmed that the fabricated samples fall within the microfiltration (MF)-ultrafiltration (UF) range of membrane separation.

Preparation of Dexamethasone-21-palmitate Incorporated Lipid Nanosphere: Physical Properties by Varying Components and Ratio of Lipid (팔미틴산덱사메타손이 봉입된 지질나노입자의 제조: 지질종류와 함량에 따른 물리적 특성)

  • Jung, Suk-Hyun;Lee, Jung-Eun;Seong, Ha-Soo;Shin, Byung-Cheol
    • Journal of Pharmaceutical Investigation
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    • v.36 no.6
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    • pp.355-361
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    • 2006
  • Intraarticular corticosteroid injections for therapy of rheumatic arthritis are administered with the aim of optimal local anti-inflammatory effect at the injection site. Since the side effects of corticosteroidal drug, dexamethasone(DEX), administered at hish dose limited the therapeutic efficacy, there was a need to design a new drug delivery system for controlled release of dexamethasone. As a prodrug for continuous therapeutic efficacy, dexamethasone-21-palmitate(DEX-PAL) was prepared via esterification of palmitoyl chloride and dexamethasone. DEX-PAL was identified by NMR and MASS analysis. DEX-PAL or DEX was entrapped in lipid nanosphere which could be prepared by using a self emulsification-solvent evaporation method. Physicochemical characteristics such as mean particle diameter, zeta potential and drug loading efficiency of the lipid nanospheres were investigated with variation of either the kind of lipid or the lipid composition. The lipid nanospheres had a mean diameter $83{\sim}95$ nm and DEX-PAL loading efficiency of up to 95%. The drug loading efficiency increased with the increase of aliphatic chain length attached to the phospholipid. The incorporation of cationic lipid was very efficient for both reducing particle size of lipid nanospheres and enhancing drug loading efficiency. The lipid nanospheres containing DEX-PAL may be a promising novel drug carrier for the controlled release of the poorly water-soluble drugs.

Solubilization of IH-901, a Novel Intestinal Metabolite of Ginseng Saponin, in Aqueous Solution (인삼사포닌의 소장내 최종대사물인 IH-901의 수용액중 가용화)

  • Kwon, Oh-Seung;Chung, Youn-Bok
    • Journal of Pharmaceutical Investigation
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    • v.34 no.5
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    • pp.385-391
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    • 2004
  • The purpose of the present study was to formulate the aqueous solution of $20-O-{\beta}-D-glucopyranosyl-20(S)-protopanaxadiol\;(IH-901)$, an intestinal bacterial metabolic derivative from Ginseng protopanaxadiol saponin. For this purpose, the effects of various solubilization agents such as cosolvents [ethanol, propylene glycol (PG), polyethylene glycol 300 (PEG 300), polyethylene glycol 400 (PEG 400), glycerin], surfactants $(Tween\;80,\;Cremophor^{\circledR}\;RH40,\;Cremophor^{\circledR}\;EL,\;Poloxamer\;407,\;Poloxamer\;188)$ and a complexation agent $[hydroxypropyl-{\beta}-cyclodextrin\;(HPBCD)]$, on the solubility of IH-90l in aqueous solution were evaluated. The solubility of IH-901 in water was under $1\;{\mu}g/ml\;at\;20^{\circ}C$. Cosolvents such as ethanol, PG, PEG 300, PEG 400 and glycerin did not enhance the solubility of IH-901 at the 0 - 40% concentration range. The solubility of IH-901 was significantly elevated by the addition of cosolvents over the 80% concentration range. On the other hand, tween 80, $Cremophor^{\circledR}\;EL,\;Cremophor^{\circledR}\;RH40$ and HPBCD showed enhanced effects on the solubility of IH-901. The enhanced effects of Poloxamer 407 or Poloxamer 188 on the IH-901 solubility were less pronounced compared with $Cremophor^{\circledR}\;EL\;or\;Cremophor^{\circledR}\;RH40$. As a results, $Cremophor^{\circledR}$ aqueous solution was selected as an optimum solvent system. The aqueous solutions containing 10% $Cremophor^{\circledR}\;EL$ and 7% $Cremophor^{\circledR}\;RH40$ were formulated as dosing solutions containing 5.0 mg/ml of IH-901 for its intravenous and oral administration, respectively. The formular showed physical stability after stored for 7 days at $4^{\circ}C$.

A Study on the Precursor of $BaTiO_3$ Synthesized in Water (수용액계에서 합성한 $BaTiO_3$의 선구물질에 관한 연구)

  • Kim, Seungwon;Huh, Woo Young;Lee, Chul
    • Analytical Science and Technology
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    • v.5 no.4
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    • pp.409-415
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    • 1992
  • Factor analysis was applied to X-ray diffraction patterns of the precursor of $BaTiO_3$. For that purpose, the precursor was synthesized in water solvent system using $Ba(NO_3)_2$ and $TiO(NO_3)_2$ as the starting materials and calcined at various temperatures. The samples obtained from the various calcined temperatures were analyzed by the X-ray diffractometer. Factor analysis was applied to the intensity data of the X-ray diffraction patterns. As the results, three factors were found and they were found to be $BaCO_3$, $BaTiO_3$ and $Ba_2TiO_4$. The relative concentrations of the three components were estimated during calcination.

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Fabrication of Biomass Based Polyethylene Furoate Nanofiber by Electrospinning (전기방사법을 이용한 바이오매스 유래 polyethylene furoate 나노섬유 제조에 관한 연구)

  • Choi, Hyun-Jin;Kim, Sun Hee;Kim, Beak-Jin;Kim, Sang Bum
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.15 no.6
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    • pp.4024-4031
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    • 2014
  • Nanofibers have attracted significant interest in many industrial fields because their high surface area and porosity. In addition, the continued use of petrochemical based polymers has caused the depletion of oil resources and accelerated the greenhouse effect by the emission of carbon dioxide. Therefore, biomass-based polymer has become a very important environmentally friendly alternative. In this study, nanofibers were fabricated by an electrospinning process using biomass based PEF(polyethylene furoate) prepared by the polymerization of 2,5-furandicaboxylic acid and ethylene glycol. Furthermore, the electrospun nanofiber was strongly affected by various parameters, such as the solvent, polymer concentration and electric field. In conclusion, nanofibers with an average fiber diameters of 200 - 700 nm could be prepared at polymer concentration of 15 wt% using HFIP, and their fiber diameter increased with increasing electric field.

Screening System for Chitin Synthase II Inhibitors from Natural Resources and its Inhibitor Prodigiosin

  • Hwang, Eui-Il;Kim, Young-Kook;Lee, Hyang-Bok;Kim, Hong-Gi;Kim, Sung-Uk
    • Journal of Microbiology and Biotechnology
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    • v.10 no.2
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    • pp.251-257
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    • 2000
  • Chitin synthases are identified as key enzymes of chitin biosynthesis in most of the fungi. Among them, chitin synthase II has been reported to be and essential enzyme in chitin biosynthesis, and exists as a membrane-bound form. To search and screen new antifungal agents from natural resources to inhibit chitin synthase II, the assay conditions were established using the enzyme isolated from Saccharomyces cerevisiae ECY38-38A(pAS6) that overproduces only chitin synthase II. This enzyme was activated only by partial proteolysis with trypsin. Its actibity reached the maximum at $80{\;}\mu\textrm{g}/ml$ of trypsin and was strongly stimulated by 2.0 mM $Co^{2+}$, 1.0 nM UDP-[$^{14}C$]-GicNAc, and 32 mM free-GlcNAc. Under these assay conditions, the highest chitin synthase II activity was observed by incubation at $30^{\circ}C$ for 90 min. However, and extremely narrow range of organic solvents up to as much as 25% of DMSO and 25% of MeOH was useful for determining optimal assay conditions. After a search or potent inhibitors of chitin synthase II from natural resources, prodigiosin was isolated from Serratia marcescens and purified by solvent extration and silica gel column chromatographies. The structure of prodigiosin was determined by UV, IR, Mass spectral, and NMR spectral analyses. Its molecular weight and formula were found to be 323 and $C_{20}H_{25}N_{3}O$, respectively. Prodigiosin ingibited chitin synthase II by 50% at the concentration of $115{\;}\mu\textrm{g}/ml$.

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Anti-proliferative and Antioxidant Activities of 1-methoxy-3-methyl-8-hydroxy-anthraquinone, a Hydroxyanthraquinoid Extrolite Produced by Amycolatopsis thermoflava strain SFMA-103

  • Kumar, C. Ganesh;Mongolla, Poornima;Chandrasekhar, Cheemalamarri;Poornachandra, Yedla;Siva, Bandi;Babu, K. Suresh;Ramakrishna, Kallaganti Venkata Siva
    • Microbiology and Biotechnology Letters
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    • v.45 no.3
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    • pp.200-208
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    • 2017
  • Actinobacteria are prolific producers of a large number of natural products with diverse biological activities. In the present study, an actinobacterium isolated from sunflower rhizosphere soil sample collected from Medak, Andhra Pradesh, South India was identified as Amycolatopsis thermoflava strain SFMA-103. A pigmented secondary metabolite in culture broth was extracted by using methanol and it was further purified by silica gel column chromatography with methanol-chloroform solvent system. Structural elucidation studies based on UV-visible, 1D and 2D-NMR, FT-IR, and mass spectroscopic analyses confirmed the structure as 1-methoxy-3-methyl-8-hydroxy-anthraquinone. It showed significant in vitro anticancer activity against lung cancer and lymphoblastic leukemia cells with $IC_{50}$ values of 10.3 and $16.98{\mu}M$, respectively. In addition, 1-methoxy-3-methyl-8-hydroxy-anthraquinone showed good free radical scavenging activity by DPPH method with an $EC_{50}$ of $18.2{\mu}g/ml$. It also showed other promising superoxide radical scavenging, nitric oxide radical scavenging and inhibition of lipid peroxidation activities. This is a first report of anti-proliferative and antioxidant activities of 1-methoxy-3-methyl-8-hydroxy-anthraquinone isolated from A. thermoflava strain SFMA-103 which may find potential application in biotechnological and pharmaceutical fields.