• Title/Summary/Keyword: high-purity

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Efficient Isolation of Dihydrophaseic acid 3'-O-β-D-Glucopyranoside from Nelumbo nucifera Seeds Using High-performance Countercurrent Chromatography and Reverse-phased High-performance Liquid Chromatography

  • Rho, Taewoong;Yoon, Kee Dong
    • Natural Product Sciences
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    • v.24 no.4
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    • pp.288-292
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    • 2018
  • High-performance countercurrent chromatography (HPCCC) coupled with reversed-phase highperformance liquid chromatography (RP-HPLC) method was developed to isolate dihydrophaseic acid 3'-O-${\beta}$-D-glucopyranoside (DHPAG) from the extract of Nelumbo nucifera seeds. Enriched DHPAG sample (2.3 g) was separated by HPCCC using ethyl acetate/n-butanol/water system (6:4:10, v/v/v, normal-phase mode, flow rate: 4.0 mL/min) to give 23.1 mg of DHPAG with purity of 88.7%. Further preparative RP-HPLC experiment gave pure DHPAG (16.3 mg, purity > 98%). The current study demonstrates that utilization of CCC method maximizes the isolation efficiency compared with that of solid-based conventional column chromatography.

Crystallization of High Purity Ammonium Meta-Tungstate for production of Ultrapure Tungsten Metal

  • Choi, Cheong-Song
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1997.10a
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    • pp.1-5
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    • 1997
  • The growth mechanism of AMT(Ammonium Meta-Tungstate) crystal was interpreted as two-step model. The contribution of the diffusion step increased with the increase of temperature, crystal size, and supersaturation. The crystal size distribution from a batch cooling crystallizer was predicted by the numerical solution of a mathematical model which uses the kinetics of nucleation and crystal growth. Temperature control of a batch crystallizer was studied using Learning control algorithm. The purity of AMT crystal producted in this investigation was above 99.99%.

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Preparation of Alumina and Amorphous Silica from Clay Minerals (점토광물로부터 알루미나 및 비정질 실리카 제조에 관한 연구)

  • 박희찬;조원제;강효경;손명모
    • Journal of the Korean Ceramic Society
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    • v.26 no.1
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    • pp.81-90
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    • 1989
  • High purity alumina and amorphous silica were prepared from Ha-dong kaolin by means of appliance of sulfuric acid. The effect of sulfuric acid concentration, reaction temperature and reaction time on the formation of aluminum sulfate was investigated. The precipitation conditions ofaluminum sulfate from the sulfuric acid solution with ethanol and ammonium hydroxide were deteremined. In the optimum condition, the conversion of aluminum oxide in kaolin to aluminum oxide powder was 85.0 percent. Alumina powder was prepared by calcination of the precipitates, and its purity was 99.0 percent.

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The Comparative Study on Zanthoxylum Peel's Impurity Tolerance Based on Pharmacopoeia by Countries (산초(山椒)의 이물허용치에 대한 각국의 약전 비교연구)

  • Park, Su-Jin;Kim, In-Rak
    • The Korea Journal of Herbology
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    • v.25 no.1
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    • pp.45-54
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    • 2010
  • Objectives : The purpose of this study is to determine the impurity tolerance of Zanthoxylum Peel. Methods : Compare with medicinal Herb Books and the Pharmacopoeia of 6 nations. Results : Current Pharmacopoeia show different Zanthoxylum Peel's Purity, such as 2.0% of seeds and fruit stalk, etc. in North Korea, 2% of seeds in Vietnam, totally 3% in China. On the other hand, Korea and Japan set the total number 26.0% including the specific numbers such as 20.0% of seeds, 5.0% of fruit stalk, 1.0% of the other foreign matter. This Zanthoxylum Peel's Purity, 26.0%, is too high compared to that of other medical matters specified by The Korean Pharmacopoeia Ninth Edition. When The Japanese Pharmacopoeia Sixth Edition firstly set the Zanthoxylum Peel's Purity, the herbal name was Fructus. However, since the part for medical usage in origin is well-ripen pericarp, not seed, the permissible level, 30.0%, is supposed to be simple error range, 3.0%. Conclusions : As a result, I think bills concerning the Zanthoxylum Peel's Purity should be revised to the total number 3.0% or specifically set the level 2.0% of seeds, 1.0% of fruit stalk, twig and so on.

Assessment of the Purity of Emodin by Quantitative Nuclear Magnetic Resonance Spectroscopy and Mass Balance

  • Park, Sojung;Choi, Yu-Jin;Do, Giang Hoang;Seo, Eun Kyoung;Hyun, Seunghun;Lee, Dongho
    • Natural Product Sciences
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    • v.25 no.3
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    • pp.222-227
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    • 2019
  • Quantitative nuclear magnetic resonance (qNMR) is a well-established method adopted by international pharmacopoeia for quantitative and purity analyses. Emodin is a type of anthraquinone, well known as the main active component of Fabaceae, Polygonaceae and Rhamnaceae. Purity analysis of emodin is usually performed by using the high-performance liquid chromatography (HPLC)-UV method. However, it cannot detect impurities such as salts, volatile matter, and trace elements. Using the qNMR method, it is possible to determine the compound content as well as the nature of the impurities. Several experimental parameters were optimized for the quantification, such as relaxation delay, spectral width, number of scans, temperature, pulse width, and acquisition time. The method was validated, and the results of the qNMR method were compared with those obtained by the HPLC and mass balance analysis methods. The qNMR method is specific, rapid, simple, and therefore, a valuable and reliable method for the purity analysis of emodin.

Hydrogen Purification by the Four-Bed Pressure Swing Adsorption Process from Steam Methane Reforming Off-Gas (4탑 PSA 공정의 의한 SMR off-gas로부터 수소 정제)

  • Yang, Se-Il;Park, Ju-Yong;Jang, Seong-Cheol;Kim, Sung-Hyun;Choi, Dae-Ki
    • 한국신재생에너지학회:학술대회논문집
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    • 2008.10a
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    • pp.383-386
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    • 2008
  • The four-bed PSA process using a layered bed of activated carbon and zeolite 5A was studied to produce a high purity hydrogen product from SMR off-gas. At a desired product purity (99.999%+), the recovery increased with decreasing the linear velocity. However, the difference of the increasing of the recovery became smaller with the decreasing of the linear velocity and then was similar from below the linear velocity 3.9 cm/s. When the adsorbents, the feed gas composition, and the operating conditions are given, the residence time is mainly a function for design of the PSA bed size. The minimum residence time exists to obtain the maximum recovery at desired product purity.

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Study on the Manufacture of High-purity Vanadium Pentoxide for VRFB Using Chelating Agents (킬레이트제를 활용한 VRFB용 고순도 오산화바나듐 제조 연구)

  • Kim, Sun Kyung;Kwon, Sukcheol;Kim, Hee Seo;Suh, Yong Jae;Yoo, Jeong Hyun;Chang, Hankwon;Jeon, Ho-SeoK;Park, In-Su
    • Resources Recycling
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    • v.31 no.2
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    • pp.20-32
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    • 2022
  • This study implemented a chelating agent (Ethylenediaminetetraacetic acid, EDTA) in purification to obtain high-purity vanadium pentoxide (V2O5) for use in VRFB (Vanadium Redox Flow Battery). V2O5 (powder) was produced through the precipitation recovery of ammonium metavanadate (NH4VO3) from a vanadium solution, which was prepared using a low-purity vanadium raw material. The initial purity of the powder was estimated to be 99.7%. However, the use of a chelating agent improved its purity up to 99.9% or higher. It was conjectured that the added chelating agent reacted with the impurity ions to form a complex, stabilizing them. This improved the selectivity for vanadium in the recovery process. However, the prepared V2O5 powder exhibited higher contents of K, Mn, Fe, Na, and Al than those in the standard counterparts, thus necessitating additional research on its impurity separation. Furthermore, the vanadium electrolyte was prepared using the high-purity V2O5 powder in a newly developed direct electrolytic process. Its analytical properties were compared with those of commercial electrolytes. Owing to the high concentration of the K, Ca, Na, Al, Mg, and Si impurities in the produced vanadium electrolyte, the purity was analyzed to be 99.97%, lower than those (99.98%) of its commercial counterparts. Thus, further research on optimizing the high-purity V2O5 powder and electrolyte manufacturing processes may yield a process capable of commercialization.

Measurement of Optical Purity for Commercially Avialable Naproxen Sold in 2013 (2013년 시판된 나프록센의 광학순도 측정)

  • Seo, Hae Chan;Song, Jung Suk;Ryoo, Sang Hyun;Lee, Sang Heon;Ryoo, Dong Hyun;Yu, Jeong Jae;Ryoo, Jae Jeong
    • Journal of the Korean Chemical Society
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    • v.58 no.2
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    • pp.179-185
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    • 2014
  • Commercial (S)-naproxen was racemized under strong basic condition. After checking the peak position of (R)- and (S)-naproxen by analysis the recemized naproxen, optical purity of 19 commercialized naproxens sold in 2013 in Korea were examined by chiral HPLC. The Chiralcel OD-H column, ChiralHyun-LE(S)-1 column and LUX-Cellulose-1 column were used as chiral stationary phases and the mixed eluent of hexane:isopropanol:acetic acid as 100:1:0.1 was used as a mobile phase with a flow rate of 1.0 mL/min. Each data was obtained from an average value of at least three different experiments for each sample and the relative standard deviation of them appeared very small. The average optical purity values obtained from three different chiral columns were very similar and the total average optical purity value (99.32%) of nineteen commercialized naproxens used in this study were larger than those of three years ago (98.17%).

Industrial-Scale Production of High-Purity Antihemophilic Factor IX from Human Plasma (사람 혈장으로부터 고순도 혈액응고 제9인자의 산업적 생산)

  • Kang, Yong;Choi, Yong-Woon;Sung, Hark-Mo;Sohn, Ki-Whan;Shin, Jeong-Sup;Kim, In-Seop
    • KSBB Journal
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    • v.23 no.1
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    • pp.37-43
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    • 2008
  • The use of antihemophilic factor IX complex has been associated with a variety of thrombotic complications, the major cause of which was the contamination of thrombogenic proteins such as vitamin K-dependent clotting factors II, VII, and X. In order to produce a commercial factor IX (GreenNine VF) free from thrombogenic potential, industrial-scale production process for high-purity factor IX from human plasma has been developed. The purification process contains cryo-precipitation, DEAE-sephadex A-50 anion-exchange chromatography, DEAE-toyopearl 650M anion-exchange column chromatography, heparin-sepharose 6FF affinity column chromatography, and CM-sepharose FF cation-exchange column chromatography. Also the process includes two viral inactivation and removal procedures, solvent/detergent treatment and nanofiltration using Viresolve NFP filter. The purification yield was 35.4%. The specific activity in the purified concentrate was 190.8 IU/mg which exceeded that in the factor IX complex (FacNine) by a factor of 48. The activities of factor II, VII, and X were not detected in GreenNine VF. SDS-PAGE analysis showed that GreenNine VF had the highest purity in comparison with commercially available high purity factor IX concentrates, Mononine, Octanyne, Berinin HS, and Immunine STIM plus 600. One batch size of the production was 2,400 vials of 250 IU product or 1,200 vials of 500 IU product from 1,600 L cryo-poor plasma.

Enantiomeric Purity Test of Bevantolol by Reversed-Phase High Performance Liquid Chromatography after Derivatization with 2,3,4,6-tetra-O-acetyl-$\beta$-D-glucopyranosyl Isothiocyanate

  • Kim, Kyeong-Ho;Heo, Sung-Young;Hong, Seon-Pyo;Lee, Beom-Chan
    • Archives of Pharmacal Research
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    • v.23 no.6
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    • pp.568-573
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    • 2000
  • A reversed-phase high-performance liquid chromatographic method was developed to determine the optical purity of bevantolol enantiomers. (S)-(-)-Menthyl chloroformate((-)-MCF), (S)-(-)-$\alpha$-methylbenzyl isocyanate((-)-MBIC) and 2,3,4,6-tetra-O-acetyl-$\beta$-D-glucopyranosyl isothiocyanate(GITC), which can react with the secondary amine group of bevantolol were investigated as chiral derivatization reagents. Among them indirect chiral HPLC method using CITC gave the best result. The derivatization proceeded quantitatively within 20 min at room temperature. Separation of the enantiomers as diastereomers was achieved by reversed-phase HPLC within 20min using ODS column. Different ratios of (S)-(-)-bevantolol and (R)-(+)-bevantolol were prepared. Enantiomeric separation of these mixtures took place on a chiralcel OD column or, after derivatization with GITC, on a ODS column. No racemization was found during the experiment. This method allowed determination of 0.05% of either enantiomer in the presence of its stereoisomer and method validation showed adequete linearity over the required range.

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