• Title/Summary/Keyword: chromatographic purification

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Chemical Studies on the Alkaloidal Constituents of Codonopsis lanceolata (더덕의 알칼로이드 성분에 관한 연구)

  • 장영경;김상열;한병훈
    • YAKHAK HOEJI
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    • v.30 no.1
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    • pp.1-7
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    • 1986
  • The alkaloid components in the root of Codonopsis lanceolata were studied. From the ether soluble alkaloid fraction, four $\beta$-carboline alkaloids were isolated in crystalline state by chromatographic purification process; comp. I mp $178^{\circ}$, isolated yield 4.5$\times$$10^{-5}%$, comp. II mp $166^{\circ}$, 6.0$\times$$10^{-5}%$, comp. III mp $164^{\circ}$, 1.8$\times$$10^{-4}%$ and comp. IV mp $197^{\circ}$, 3.5$\times$$10^{-5}%$. They were identified by spectral analysis and by total synthesis as being a new component $N_9$-formylharman, and already known components in other plant 1-carbomethoxy-$\beta$-carboline, perlolyrine and norharman.

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Studies on the Constituents of Rhamnella frangulioides (까마귀베개뿌리의 성분에 관한 연구)

  • Yoo, Seung-Jo;Song, Kyung-Shik;Kwak, Jong-Hwan;Han, Byung-Hoon;Ryu, Jae-Ha
    • Korean Journal of Pharmacognosy
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    • v.20 no.3
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    • pp.147-148
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    • 1989
  • From the root of Rhamnella frangulioides(=Microrhamnus frangulioides), three compounds (Comp. I ; $mp\;140{\sim}142^{\circ},\;Comp.\;II\;;\;mp\;196^{\circ},\;Comp.\;III\;;\;mp\;136{\sim}138^{\circ})$ were isolated by silica gel column chromatographic purification which were identified as ${\beta}-sitosterol$, chrysophanol, 1-methyl-2-carboxymethyl-3-methoxy-4,8-dihydroxy andthraquinone, respectively by spectral analysis.

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Various Bioactivities of Two Polyphenolic Compounds from the Brown Alga Grateoupia elliptica

  • Kim, Eun-Sook;Kim, Chan-Sook;Lee, Bong-Ho;Choi, Byoung-Wook;Ryu, Geon-Seek
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.190.2-190.2
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    • 2003
  • In the course of search for various bioactive compounds from marine algae, we found strong antioxidant activity of the methanolic extract of the brown alga G. elliptica. Chromatographic purification [ODS flash, gel-filtration on Sephadex LH-20, HPLC] of the BuOH layer of the methanolic extract afforded two known polyphenolic compounds, 6,6'-bieckol (1) and dieckol (2). Compound 1 showed acetylcholinesterase (AChE) and butyrylcholinesterase (BuChE) inhibitory activities, free radical scavenging activity on DPPH (1,1-diphenyl-2-picryl-hydazyl) with IC$\_$50/ values of 91.2, 45.6 and 15.5 $\mu\textrm{g}$/$m\ell$, respectively. (omitted)

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A Study on the Purification Process of Methyl Fructoside by Liquid Chromatography (액체 크로마토그래피에 의한 메틸프룩토시드의 분리공정 연구)

  • 허주형;유인상김해성
    • KSBB Journal
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    • v.11 no.5
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    • pp.529-535
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    • 1996
  • Methyl frucloside was purified from the aqueous sugar/methyl fructoside solution by liquid chromatography using Amberlite IRA-900, strong anion-exchange resin. The optimum operating conditions, resolution and productivity of methyl fructoside were discussed to evaluate the practical feasibility of the proposed chromatographic separation process of methyl fructoside which is useful as a new starting material for sugar ester synthesis. The linear chromatography model with HETP was well applied to the chromatographic separation process of methyl fructoside and the theoretical solution successfully predicted the elution chromatogram of methyl fructoside and sucrose at different superficial linear velocity of eluent for rectangular feed with different loading volume of packed bed. The optimum operating conditions were found to be 75% with the loading volume of packed bed at 1.13 cm/min of the superficial linear velocity at $60^{\circ}C$, and gave the productivity of methyl fructoside of 7 mg/g-resin/h with the resolution of 1.1.

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Development of Miniaturized Automatic Chromatography System for validation Study of Chromatographic Resin lifetime (크로마토그래피 담체의 수멍을 검증하기 위한 자동화 미니 크로마토그래피 시스템 개발)

  • 박재하;서창우
    • KSBB Journal
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    • v.17 no.4
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    • pp.326-332
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    • 2002
  • The quality of biopharmaceutical proteins is strongly affected by a manufacturing process employed to produce Et, and thus validation of the manufacturing bioprocess is a very important issue. Chromatography is probably the most widely used bioprocess unit operation for protein purification. In this study, a miniaturized automatic chromatography system was designed and constructed for scale-down studies for process chromatography validation. This system, named MiniValChrom, has the following features: automatic and repeated operation, flexible sequences and intervals among the steps, on-line and real-time monitoring and control, method files savings, etc. Using the MiniValChrom, we peformed a case study of an abbreviated experiment to estimate chromatographic resin lifetime. BSA (bovine serum albumin) and Cibacron Blue 3G-A were used as the model protein and the resin, respectively. The resin deterioration was evaluated by determining and monitoring the HETP and NTP values from the chromatograms every 5 cycles. It was observed that the HETP and the NTP values were changed by 9% after 15 cycles. The resin lifetime validation could be completed by repeating this experiment until the HETP value reached a predetermined value. The MiniValChrom's concept and the protocol suggested in this study can serve as a rapid and economical tool for the validation studies of bioprocess chromatography system.

Adsorption Column Chromatography for Simultaneous Determination of Multi-pesticide Residues (잔류농약 다성분 동시분석을 위한 흡착 크로마토그래피의 적용)

  • Kim, Chan-Sub;Ihm, Yang-Bin;Choi, Ju-Hyun;Lee, Kyoung-Mi;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
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    • v.14 no.4
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    • pp.347-360
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    • 2010
  • In order to develop the multi-residue purification method for 180 pesticides commonly used in Korea, many analytical methods on individual and multi- pesticide residues in the agricultural commodities and food product were examined. Through the modification of adsorption chromatographic methods used in Europe, the United States and Korea, the Florisil and silica-gel chromatographic systems were developed. Through these purification systems, elution profiles for all pesticides were examined. As the results, 145 pesticides were recovered in the range of 70-120% in Florisil clean-up system. The distribution of pesticides in the elution profile was 12 pesticides in the first fraction, 76 pesticides in the second fraction, 81 pesticides in the third fraction, 60 pesticides in the fourth fraction and 30 pesticides in the last fraction. And, in silica-gel system, 137 pesticides were recovered in the range of 70~120%. The distribution of pesticides in the elution profile was 22 pesticides in the first fraction, 59 pesticides in the second fraction, 102 pesticides in the third fraction, 46 pesticides in the fourth fraction and 8 pesticides in the last fraction.

Purification of Paclitaxel and Its Derivatives by Supercritical Fluid Chromatography(SFC) (초임계 유체 크로마토그래피(SFC) 방법에 의한 Paclitaxel 및 그 유도체의 분리 정제)

  • 조병관;변상요
    • KSBB Journal
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    • v.14 no.1
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    • pp.17-23
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    • 1999
  • Studies were carried out to elucidate the effects of pressure, temperature and mobile phase composition on supercritical $CO_2$ chromatographic separations of paclitaxel, baccatin III, 10-deacetyl baccatin III, 7-epi-10-deacetyltaxol, cephalomanine, and 10-deacetyltaxol. High resolutions of paclitaxel, 10-deacetylbaccatin III, 10-deacetyltaxol were observed with optimized pressure, temperature, and mobile phase composition. The highest resolution between paclitaxel and 10-deacetylbaccain III was observed at 275 kg/$\textrm{cm}^2$, $40^{\circ}C$ with the mobile phase composition of gradient mixture of 3.9-3.6 mL/min $CO_2$, 0.1-0.4 mL/min methanol for 20 min. Resolutions of baccatin III, capalomannine, and 7-epi-10-deacetyltaxol were found to be low in this study. On-line coupled SFE/SFC process was applied to isolate paclitaxel from yew tree powder. As a consequence, paclitaxel with a purity of 95% was obtained with a recovery yield of 38%.

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Extraction and Purification of EGCG(Epigallocatechin Gallate) from Green Tea (녹차로부터 EGCG(Epigallocatechin Gallate)의 추출 및 정제)

  • Gang, Ji-Hun;Park, Yeong-Gwang;Jeong, Seong-Taek;No, Gyeong-Ho
    • KSBB Journal
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    • v.14 no.5
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    • pp.517-522
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    • 1999
  • A green tea used in this experiment was cultivated at Bosung (Chonnam) and purchased from a domestic market. The extract at 5$0^{\circ}C$ water from the powder of green tea partitioned with chloroform and ethyl acetate. The resulting solution was further purified with a chromatographic column (4.6$\times$250 mm, 15${\mu}{\textrm}{m}$, Lichrospher 100RP-18). Finally separation was achieved on a $\mu$-Bondapak $C_18$(3.9$\times$300mm, 10${\mu}{\textrm}{m}$) column. The elution order of the catechin compounds contained in the green tea was EGC(Epigallocatechin, C(catechin), EC(Epicatechin), EGCG(Epigallocatechin Gallate) and ECG(Epicatechin Gallate). From the experimental results the mobile phase for isolating EGCG from the extract consisted of 0.1% acetic acid in water/acetonitrile, 87/13%(v/v). The flow rate of mobile phase was 1.0 $m\ell$/min, and UV wavelength was fixed at 280 nm. 121.3 mg of EGCG, higher than 98% of purity, was obtained from 5 g of dry green tea.

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Purification and Characterization of Antioxidative Peptides from Bovine Skin

  • Kim, Se-Kwon;Kim, Yong-Tae;Byun, Hee-Guk;Park, Pyo-Jam;Ito, Hisashi
    • BMB Reports
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    • v.34 no.3
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    • pp.219-224
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    • 2001
  • To identify the antioxidative peptides in the gelatin hydrolysate of bovine skin, the gelatin was hydrolyzed with serial digestions in the order of Alcalase, pronase E, and collagenase using a three-step recycling membrane reactor. The second enzymatic hydrolysate (hydrolyzed with pronase E) was composed of peptides ranging from 1.5 to 4.5 kDa, and showed the highest antioxidative activity, as determined by the thiobarbituric acid method. Three different peptides were purified from the second hydrolysate using consecutive chromatographic methods. This included gel filtration on a Sephadex G-25 column, ion-exchange chromatography on a SP-Sephadex C-25 column, and high-performance liquid chromatography on an octadecylsilane chloride column. The isolated peptides were composed of 9 or 10 amino acid residues. They are: Gly-Glu-Hyp-Gly-Pro-Hyp-Gly-Ala-Hyp (PI), Gly-ProHyp-Gly-Pro-Hyp-Gly-Pro-Hyp-Gly (PII), and Gly-ProHyp-Gly-Pro-Hyp-Gly-Pro-Hyp (PIII), as characterized by Edman degradation and fast-atom bombardment mass spectrometry. The antioxidative activities of the purified peptides were measured using the thiobarbituric acid method, and the cell viability with a methylthiazol tetrazolium assay The results showed that PII had potent antioxidative activity on peroxidation of linoleic acid. Moreover, the cell viability of cultured liver cells was significantly enhanced by the addition of the peptide. These results suggest that the purified peptide, PII, from the gelatin hydrolysate of bovine skin is a natural antioxidant, which has potent antioxidative activity.

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Purification and Characterization of an Antioxidant Protein from Fertilized Eggs

  • Yang, Shaohua;Tang, Zhengjiang;Tang, ShanShan;Zhang, Tingfang;Tang, Fei;Wu, Yu;Wang, Ying;Wang, Lu Lu;Liu, Guoqing
    • Food Science of Animal Resources
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    • v.36 no.6
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    • pp.791-798
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    • 2016
  • Free radicals may attack cells or tissue, leading to chronic diseases, and antioxidant consumption is potentially useful for removing free radicals. Egg proteins may be used as potential sources of antioxidant considering their ability of scavenging free radicals to apply for food or cosmetics industry. In this study, we obtained a natural antioxidant protein from fertilized eggs, which was a dietary supplement in some Asian countries. Meanwhile, antioxidant activities of these proteins were evaluated using different oxidation systems. With increasing incubation time, the antioxidant activity of these proteins increased during 15 d of incubation. The samples on day 15 were performed for isolation of antioxidant protein. The protein, named P4-1 (MW, 45 kDa), was isolated and purified by consecutive chromatographic methods. P4-1 contained 17 amino acids, which was determined by liquid chromatography-mass spectrometry and Amino Acid Analyzer. Moreover, the amino acid sequence was highly similar to that of ovalbumin. Differential scanning calorimetry showed that the denaturation temperature of P4-1 was $57.16^{\circ}C$. Furthermore, P4-1 suggested high oxygen radical-absorbance activity in ${\cdot}OH$ assays, and its antioxidant activity was stable at $30-50^{\circ}C$ in acidic and neutral pH. Thus, these results revealed that P4-1 may be a potential resource as a natural antioxidant.