• Natural Product Sciences
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• 제24권4호
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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.

• 한국결정성장학회:학술대회논문집
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• 한국결정성장학회 1997년도 Proceedings of the 13th KACG Technical Meeting `97 Industrial Crystallization Symposium(ICS)-Doosan Resort, Chunchon, October 30-31, 1997
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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%.

• 한국세라믹학회지
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• 제26권1호
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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.

• 대한본초학회지
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• 제25권1호
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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.

• Natural Product Sciences
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• 제25권3호
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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.

• 한국신재생에너지학회:학술대회논문집
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• 한국신재생에너지학회 2008년도 추계학술대회 논문집
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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.

• 자원리싸이클링
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• 제31권2호
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• pp.20-32
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• 2022

본 연구에서는 VRFB용 고순도 오산화바나듐을 제조하기 위한 불순물 분리 정제 공정에서 킬레이트제(EDTA)의 영향을 조사하였다. 저순도 바나듐 원료를 이용하여 제조된 바나듐 용액으로부터 NH₄VO₃ 을 침전 회수하여 제조된 최종 V₂O₅ 분말의 순도는 99.7%로 분석되었지만 NH₄VO₃ 침전 회수 공정에서 킬레이트제를 첨가한 경우 최종 V₂O₅ 분말 순도가 99.9% 이상으로 향상되었다. 이러한 결과는 첨가된 킬레이트제가 불순물 이온과 반응하여 complex를 형성하고 불순물 이온이 안정화되기 때문에 침전 회수 공정에서 바나듐에 대한 선택성이 향상된 것으로 판단된다. 하지만 제조된 V₂O₅ 분말내에는 불순물 규격 대비 K, Mn, Fe, Na 및 Al 함유량이 높아 추가적인 불순물 정제 연구가 필요하였다. 고순도 V₂O₅ 분말을 새롭게 개발된 직접 전해공정에 적용하여 바나듐 전해액을 제조하였고 이의 특성을 상용 전해액과 비교 분석하였다. 제조된 바나듐 전해액의 순도는 불순물 K, Ca, Na, Al, Mg 및 Si 성분의 높은 함량으로 인하여 상용 전해액의 순도 99.98%보다 낮은 99.97%로 분석되었다. 따라서 고순도 V₂O₅ 분말 및 전해액 제조 공정의 불순물 분리 정제에 대한 추가적인 최적화 연구가 수행된다면 상용화가 가능한 공정이 개발될 것으로 기대된다.

• 대한화학회지
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• 제58권2호
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• pp.179-185
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• 2014

시판되는 (S)-naproxen을 강염기 조건에서 라세미화하였다. 라세미화된 naproxen 시료를 분석하여 (R)- 및 (S)-naproxen의 피이크 위치를 확인한 후, 2013년 국내에서 시판된 19개 naproxen의 광학순도를 키랄 HPLC로 조사하였다. Chiralcel OD-H 칼럼과 ChiralHyun-LE(S)-1 칼럼 및 LUX-Cellulose-1 칼럼을 키랄 정지상으로 사용하였고, hexane:isopropanol:acetic acid가 100:1:0.1로 혼합된 용액을 전개용매로 사용하여 흐름속도 1.0 mL/min에서 분석하였다. 각 시료를 최소 3회 이상 분석하여 얻은 평균값을 각각 계산하여 데이터로 이용하였고, 이들의 상대표준편차도 계산하여 그 값이 아주 작게 나타난 것을 확인하였다. 세 종류의 다른 칼럼에서 각각 측정한 광학순도 값이 서로 아주 유사한 값을 보여주었으며, 측정된 naproxen의 광학순도는 이들의 광학순도 데이터가 처음 보고된 2010년 시료의 광학순도 평균값인 98.17%에 비해 높은 99.32%를 보였다.

• KSBB Journal
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• 제23권1호
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• pp.37-43
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• 2008

(주)녹십자는 1986년 "훽나인"을 B형 혈우병 치료제로 제조품목허가를 받아 B형 혈우병치료제 공급을 시작하였다. 또한 1991년 New York Blood Center에서 selvent/detergent 바이러스 불활화 방법을 도입하여 제조공정에 추가한 후 혈액유래 바이러스로부터 안전한 제품을 생산하여 왔다. 하지만 이 제품은 혈액응고 제2인자, 제7인자, 제10인자가 함유된 제9인자 복합체로, 정맥 혈전증과 파종성 혈관내응고병증 같은 혈전형성 부작용이 일어날 가능성이 있어, 훽나인보다 순도, 유효성, 바이러스 안전성이 우수한 제품의 개발이 필요하였다. 이를 위해 고순도 제9인자 제제인 "GreenNine VF" 제조공정을 개발하였다. GreenNine VF 제조공정은 기존의 훽나인 생산 공정에 heparin 친화성 크로마토그래피와 양이온 크로마토그래피가 추가된 공정으로, 바이러스 안전성을 증진시키기 위한 바이러스 필터 공정도 포함하고 있다. 이러한 공정에 의해서 산업적 규모로 생산된 GreenNine VF는 훽나인에 비해 순도와 바이러스 안전성이 월등히 높은 것으로 확인되었다. 또한 고순도 혈액응고 제9인자 제제인 Mononine, Octanyne, Berinin HS, Immunine STIM plus 600보다 순도가 더 높았다. Cryo-poor plasma 1,600 L를 원료로 사용했을 때 1 batch 당 250IU 분병제품 2,400병 이상, 500 IU 분병제품 1,200병 이상을 생산할 수 있었다.

• Archives of Pharmacal Research
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• 제23권6호
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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.