• 제목/요약/키워드: Preparative Chromatography

검색결과 246건 처리시간 0.023초

붉노랑상사화 인경으로부터 살초활성 물질의 분리 (Isolation of Herbicidal Substances from Bulbs of Lycoris flavescens M.Y.Kim & S.T.Lee)

  • 이동구;김건우
    • 한국잡초학회지
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    • 제31권4호
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    • pp.330-339
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    • 2011
  • 연구는 붉노랑상사화 인경에 함유된 살초활성 물질을 분리하여 살초활성을 평가하고 그 화학구조를 구명하고자 수행되었다. Silica gel flash column chromatography, preparative TLC, HPLC 등 일련의 크로마토그래피법들을 통해 붉노랑상사화 인경의 MeOH 추출물을 분리 정제하였다. HPLC에 의해 최종 획득된 활성분획에 대한 GC/MS 분석 결과, galanthine (galanthan-1-ol)과 isoquinoline alkaloid인 montanine ($O^2$-methyl pancracine)이 동정되었다. Montanine은 $20{\mu}g\;mL^{-1}$ 농도에서 돌피 유묘의 생장을 거의 100% 억제시키는 것으로 나타났다. 한편, 붉노랑상사화 인경의 MeOH 추출물은 $1,000{\mu}g\;mL^{-1}$ 에서 대조구에 비해 화영벼 유묘의 신초와 유근의 생장을 각각 약 3.1% 및 8.3% 억제하였다.

잣의 향기성분(香氣成分)에 관한 연구(硏究) (Volatile Components of Pinenut)

  • 김용갑;정규능;석정심;촌목반
    • 한국식품과학회지
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    • 제18권2호
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    • pp.105-109
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    • 1986
  • 잣의 향기성분(香氣成分)을 추출(抽出)하는데 우선 Maillard생성물(生成物)의 영향을 피하기 위하여 Soxhlet장치(裝置)에 의한 추출후(抽出後), 수증기증류(水蒸氣蒸溜) 연속추출법(蓮續抽出法)에 의해 추출(抽出)했다. 이 추출물은 다시 Preparative, TLC에 의해 4부분(部分)으로 나누고, 이 모든 fractions을 FID/FTD capillary GC로 동시(同時) 검출(檢出)하고. GC/MS에 의해 109성분(成分)을 동정(同定)했다. 관능기별(官能基別)로 보면 탄화수소(炭化水素) 26성분(成分), aldehydes류(類) 16성분(成分), alcohols류(類) 31성분(成分), ketones류(類) 12성분(成分), esters류(類) 17성분(成分), 산류(酸類) 2성분(成分), 대기(坮基) 11성분(成分), 기타 3성분(成分)이었다.

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Streptomyces fradiae에서 분리된 Aspartate Aminotransferase의 특성 (Characterization of Aspartate Aminotransferase Purified from Streptomyces fradiae)

  • Lee, Sang-Hee;Lee, Kye-Joon
    • 미생물학회지
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    • 제31권3호
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    • pp.237-244
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    • 1993
  • Aspartate aminotransferase (ASAT) (L-aspartate : 2-oxyoglutarate, EC 2.6. 1. 1.) from Streptomyces fradiae NRRL 2702 has been purified by acetone precipitation, DEAE-cellulose, hydroxyapatite, and preparative electrophoresis (Prep cell), of which the last was the most effective step in the purification of ASAT. The molecular mass was estimated to be 54,000 dalton by SDS-PAGE and 120,000 dalton by gel filtration chromatography. Preparative isoelectric focusing of purified ASAT resulted in one polypeptide band with a pI of 4.2, showing homogeneity and indicating that the enzyme is composed of two identical subunits. The enzyme was specific for L-aspartate as an amino donor ; the $K_{m}$ values were determined to be 2.7 mM for L-aspartate, 0.7 mM for 2-oxoglutarate, 12.8 mM for L-glutamate, and 0.15 mM for oxaloacetate. The enzyme was relatively heat-stable, having maximum activity at 55.deg.C, and it had a broad pH optimum ranging from 5.5 to 8.0. The activity of the purified enzyme was not inhibited by ammonium ions. This paper reports the first purification and characterization of the aspartate aminotransferase from a species of Streptomyces.s.

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고성능 액체 크로마토그래피에 의한 다당 유도체의 키랄 고정상에서 플록세틴의 새롭게 개발된 분석 및 반분취의 광학분리 (A Newly Developed Analytical and Semi-preparative Enantiomer Separation of Fluoxetine using Polysaccharide-derived Chiral Stationary Phases by High Performance Liquid Chromatography)

  • 김석진;남경욱;박보현;이스람 포크롤;이원재
    • KSBB Journal
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    • 제31권3호
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    • pp.186-191
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    • 2016
  • A liquid chromatographic method for the enantiomer separation of fluoxetine was performed using covalently bonded and coated type polysaccharide-derived chiral stationary phases (CSPs). The degree of enantioseparation is affected by the used CSPs and mobile phases. The performance of Chiralpak IC was superior to the other CSPs used in this study. Out of various solvent composition and additives, the greatest separation and resolution was observed using Chiralpak IC with mobile phase of 2-propanol in hexane with diethylamine as an additive. Semi-preparative separation of fluoxetine was performed on the analytical Chiralpak IC column to obtain (R)- and (S)-fluoxetine enantiomer with high chemical and optical purity. From the overall study, the developed liquid chromatographic method on polysaccharide-derived CSPs is expected to be very useful for the enantiomer separation of fluoxetine.

다양한 정제방법에 의한 전기영동용 한천유래 아가로즈의 제조 및 DNA분리 특성 (Preparation of Agarose from Gelidium amansii for Gel Electrophoresis using Various Purification Methods and Its Resolution Characteristics for DNA)

  • 도정룡;오세욱
    • 한국식품과학회지
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    • 제31권1호
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    • pp.110-114
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    • 1999
  • 제주도산 우뭇가사리로부터 agar를 제조하여 분석용 등급의 agarose 제조를 위하여 cetylpyridium chloride (CPC), polyethylene glycol (PEG), chitosan을 처리하여 agaropectin을 제거하여 agarose를 분리, 정제하였다. 3가지 방법중 chitosan을 처리하여 정제한 agarose는 황산기 함량이 가장 낮았으며, electroendosomosis도 가장 낮은 수치를 나타내어 분석용 agarose 제조를 위한 가장 효율적인 방법으로 나타났으며 실제 DNA 전기영동 실험에서도 가장 우수한 resolution을 나타내었으며 교차면역 전기영동에서도 시판되고 있는 제품에 비하여 품질이 양호함을 알 수 있었다.

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Antioxidant and α-Glucosidase Inhibitory Activities of the Extract from Sparganium stoloniferum Buch.-Ham. Root and Its Constituent Compounds

  • Xu, Ming Lu;Wang, Lan;Hu, Jian He;Wang, Myeong-Hyeon
    • Preventive Nutrition and Food Science
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    • 제14권4호
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    • pp.354-357
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    • 2009
  • Three compounds, vanillic acid, p-hydroxylcinnamic acid, p-hydroxybenzaldehyde have been isolated from the ethylacetate extract of Sparganium stoloniferum Buch.-Ham roots using silica gel open column chromatography, preparative thin-layer chromatography (pTLC) and reverse phase high performance liquid chromatography. The structures of the compounds were established on the basis of IR, extensive 1D NMR, and MS analyses. The ethylacetate (EtOAc) extract, vanillic acid, and p-hydroxybenzaldehyde showed $\alpha$-glucosidase inhibition activity of 72.71%, 20.13%, and 30.42%, at the concentration of 10 ${\mu}g/mL$, respectively. The EtOAc extract exhibited strong antioxidant activity with an $IC_50$ value of 24.37 ${\mu}g/mL$ against DPPH radical scavenging activity, the vanillic acid, p-hydroxylcinnamic acid, and p-hydroxybenzaldehyde with an $IC_50$ value of 2.10 ${\mu}M$, 1.59 ${\mu}M$, and 2.72 ${\mu}M$ against DPPH, respectively.

Chemical Constituents of the Culture Broth of Phellinus linteus and Their Antioxidant Activity

  • Lee, Myeong-Seok;Hwang, Byung Soon;Lee, In-Kyoung;Seo, Geon-Sik;Yun, Bong-Sik
    • Mycobiology
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    • 제43권1호
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    • pp.43-48
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    • 2015
  • The medicinal fungus Phellinus linteus, in the family Hymenochaetaceae, has been used as a traditional medicine for the treatment of various diseases. In this study, the chemical constituents of the culture broth of P. linteus were investigated. P. linteus was cultured in potato dextrose broth medium, and the culture broth was extracted with ethyl acetate. The ethyl acetate-soluble portion was concentrated and subjected to ODS column chromatography, followed by Sephadex LH-20 column chromatography. Six compounds (1~6) were purified by preparative reversed-phase high-performance liquid chromatography. Spectroscopic methods identified their structures as caffeic acid (1), inotilone (2), 4-(3,4-dihydroxyphenyl)-3-buten-2-one (3), phellilane H (4), (2E,4E)-(+)-4'-hydroxy-${\gamma}$-ionylideneacetic acid (5), and (2E,4E)-${\gamma}$-ionylideneacetic acid (6). Compounds 1, 2, and 3 exhibited potent dose-dependent antioxidant activity.

영지의 항산화성 물질에 관한 연구 (Studies on Antioxidative Substances of Ganoderma lucidum)

  • 정동옥
    • 한국식품과학회지
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    • 제24권5호
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    • pp.497-503
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    • 1992
  • 영지 추출액의 항산화 활성을 thiocyanate method, TBA method, weighing method를 이용하여 검색한 결과 n-hexane 추출물, methanol 추출물에서 항산화활성이 나타났으며 그 중에서 n-hexane 추출물의 fraction V와 methanol 추출물의 methanol 불용성 fraction II에서 강한 활성을 나타내었다. 이들 항산화 활성을 나타내는 fraction 5와 fraction II를 rat의 간 균질액을 이용한 항산화 활성 검색에서 과산화 지질 생성억제를 TBA값으로 나타내어 inhibition ratio(I.R.)를 산출하였으며 그 결과 n-hexane 추출물의 fraction V는 l5%, methanol 추출물의 methanol 불용성 fraction II는 54.6%의 억제율을 나타내었다 이는 rat의 간 mitochondria에서 과산화지질 생성 억제율이 영지의 물 추출물은 16%, acetone 추출물은 23%인 것에 비하여 약간 높았으나, microsome에서 과산화지질 생성 억제율이 물 추출물은 44%, acetone 추출물은 75%인 것에 비하여 다소 낮은 활성을 보여주었다.

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Resolution of β-Amino Acids on a Chiral Stationary Phase Based on (+)-(18-Crown-6)-2,3,11,12-tetracarboxilic Acid without Extra Free Aminopropyl Groups on Silica Surface

  • Hyun, Myung- Ho;Choi, Hee-Jung;Kang, Bu-Sung;Tan, Guang-Hui;Cho, Yoon-Jae
    • Bulletin of the Korean Chemical Society
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    • 제27권11호
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    • pp.1775-1779
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    • 2006
  • A liquid chromatographic chiral stationary phase (CSP) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxilic acid without extra free aminopropyl groups on silica surface has been demonstrated to be quite effective for the resolution of various $\beta$-amino acids. The retention factors ($k_1$) for the resolution of $\beta$-amino acids on the CSP were quite large and the large retention factors might be quite attractive along with the reasonable separation factors ($\alpha$) for preparative scale enantioselective chromatography. The large retention factors on the CSP were found to be reduced effectively by adding ammonium ion to mobile phase without sacrificing the chiral recognition efficiency of the CSP. Consequently, the CSP is also quite applicable for use in analytical enantioselective chromatography.

Purification and Characterization of Iron-Containing Superoxide Dismutase from Lentinus edodes

  • Park, Sang-Shin;Hwang, Soo-Myung
    • Journal of Microbiology and Biotechnology
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    • 제9권6호
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    • pp.854-860
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    • 1999
  • Superoxide dismutase (SOD) was purified to homogeneity from fruiting bodies of edible mushroom, Lentinus edodes, by ammonium sulfate precipitation, diethylaminoethyl (DEAE)-Sepharose FF ion-exchange chromatography, Sephacryl S-200 gel filtration chromatography, and preparative PAGE. The molecular weight of the purified enzyme was estimated to be approximately 54 kDa by gel filtration chromatography, and the enzyme was shown to be consisted of two identical subunits of molecular weight 27 kDa by SDS-PAGE. The isoelectric point of the enzyme was 4.9 as determined by isoelectric focusing. The enzyme had optimal pH and temperature of pH 8.0 and $20^{\circ}C$, respectively. The activity of the enzyme was inhibited by hydrogen peroxide, but inhibited less by cyanide and azide. The native enzyme was found to contain 0.89g-atom of iron, 0.75g-atom of zinc, and 0.46g-atom of copper per mol of enzyme. Analysis of amino acids composition revealed that the SOD from L. edodes contained a relatively large amount of glutamic acid/glutamine, proline, cysteine, isoleucine, and leucine, but only a small amount of aspartic acid/asparagine, tyrosine, and tryptophan when compared to the other iron-containing SODs.

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