• Title/Summary/Keyword: 칼럼 크로마토그래피

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Measurement of optical purity for commercial naproxen by chiral HPLC (키랄 크로마토그래피에 의한 시판되는 나프록센의 광학순도 측정)

  • Yu, Jeong-Jae;Lee, Won-Doo;Ryoo, Jae-Jeong
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.360-367
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    • 2011
  • Optical purities of 10 commercialized naproxens prepared from eight Korean drug companies were examined by an optimized chiral HPLC condition. The Chiralcel OD-H column and ChiralHyun-LE(S)-1 column were used as chiral stationary phases and the mixed eluent of hexane/isopropanol/acetic acid as 100:2.85:0.1 was used as a mobile phase for effective enantioseparation. Optical purity values of most samples were higher than 97 percents, only one of them was about 95 percents. The average relative standard deviation of them appeared very small (0.034%).

Visual Demonstration of Simulated Moving Bed (Simulated Moving Bed Chromatography의 시각적 설명)

  • Oh, Nan Suk;Lee, Chong-Ho;Kim, Jin Il;Koo, Yoon-Mo
    • Korean Chemical Engineering Research
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    • v.43 no.3
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    • pp.360-365
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    • 2005
  • SMB (simulated moving bed) is a continuous chromatographic process by shifting periodically port position. Binary of mixture, Blue dextran and Orange G, was separated by SMB. These components have unique color individually, that is, Blue dextran is blue and Orange G is orange. It is easy to understand SMB process by observing the shift of color changes in SMB. These components was not adsorbed to stationary phase and isolated by difference of size exclusion factor. Mass transfer coefficient was determined by single pulse test under several flow rate conditions. Operation condition was obtained by standing wave theory and optimized for high purities in extract and raffinate streams. Experiment was performed in open loop 4 zone (2-2-2-2) SMB. There are several advantages in open loop SMB, where extract is product for high purity. It is also easy to control flow rate and monitor experimental state during operation. Experimental, extract and raffinate history is well fitted with simulation results, however, column concentration profile is a little different from simulation results. Purities were 99.5% for extract and 98.9% for raffinate and extract and raffinate yields were obtained as 98.9% and 99.4% respectively.

Isolation and Purification of DHA from Skipjack Orbital Tissue Oil (가다랭이 안와조직으로부터 DHA의 추출 및 정제)

  • JEONG Bo-Young
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.26 no.6
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    • pp.529-537
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    • 1993
  • Several methods were examined for purification of docosahexaenoic acid (DHA, 22:6n-3) from skipjack Euthynnus pelamis orbital tissue oil, a marine by-product, and a modified method for isolation of a high purity DHA was proposed. Skipjack orbital tissue contained $55.4\%$ of total lipid(TL), and DHA accounted for $23.7\%$ of the TL. Application of low-temperature crystallization and urea inclusion compound methods to the orbital fatty acid mixture resulted in increases of DHA concentrations to approximately $46\%\;and\;61\%$, respectively. These methods were suitable for large production of DHA with relative low purity because of the simple purification procedure. DHA of approximately $74\%$ in purity was obtained by silver nitrate aqueous solution method, but the method gave a very low recovery($<10\%$). Silver nitrate-impregnated silica column chromatography was suitable for purification of a high purity DHA(purity, $>98\%$ and recovery, $>90\%$) A modified method, silver nitrate-impregnated silica column chromatography combined with low-temperature crystallization(two step purication method) was proposed as the most effective method to obtain DHA with high purity($99.9\%$) from the skipjack orbital oil.

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Extractives from the leaves of Chamaecyparis obtusa Endlicher (편백나무(Chamaecyparis obtusa Endlicher) 잎의 추출성분)

  • Lee, Sang-Keug;Kim, Jin-Kyu;Ham, Yeon-Ho;Bae, Young-Soo
    • Journal of Forest and Environmental Science
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    • v.18 no.1
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    • pp.53-60
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    • 2001
  • 2kg of the dried leaves of chamaecyparis obtusa Endlicher were ground, extracted with acetone-$H_2O$(7:3, v/v), concentrated, and fractionated with a series of hexane, $CH_2Cl_2$, EtOAc and water on a separatory funnel. Each fraction was freeze dried to give dark-brown powder and a EtOAc soluble portion of the powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. Spectrometric analyses such as NMR and FAB-MS including TLC were performed to characterize the structures of the isolated compounds. The leaves of chamaecyparis obtusa Endlicher contained a large amount of taxifolin-3-O-${\beta}$-D-xylopyranoside and (+)-catechin in addition to a small amount of quercetin-3-O-${\alpha}$-L-rhamnopyranoside.

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Extractives from the Allium victorials (산마늘(Allium victorialis)의 추출성분)

  • Lee, Hak-Ju;Lee, Sang-Keug;Choi, Yun-Jeong;Jo, Hyun-Jin;Kang, Ha-Young;Lee, Sung-Suk;Choi, Don-Ha
    • Journal of Korean Society of Forest Science
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    • v.96 no.6
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    • pp.620-624
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    • 2007
  • Allium victorials var. platyphyllum were ground, extracted with 95% EtOH, concentrated, and fractionated with a series of n-hexane, methylene chloride, ethyl acetate, butanol and water on a separatory funnel. A portion of ethyl acetate soluble fraction was chromatographed on a Sephadex LH-20 and silica gel column using various solvent system as eluents. The isolated compounds were identified by TLC, $^1H-$, $^{13}C$-NMR, HMBC and EI-MS. Astragalin (compound 1), kaempferol (compound 2), quercetin (compound 3), ferulic acid (compound 4) were isolated from the ethyl acetate soluble fraction of A. victorials.

Antibacterial Activities of Galla Rhois Extracts against Fish Pathogenic Bacteria (오배자 추출물의 어병 세균에 대한 항균 효능)

  • Choi, Hye-Sung;Kim, Jin-Sook;Jang, Dae-Sik;Yu, Young-Beob;Kim, Yi-Cheong;Lee, Joo-Seok
    • Journal of fish pathology
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    • v.18 no.3
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    • pp.239-245
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    • 2005
  • Galla Rhois was extracted with various solvents such as ethyl alcohol, ethyl acetate, n-hexane, and n-butyl alcohol, and antibacterial activity of the extracts were also tested. The ethyl acetate extracted Galla Rhois showed high antibacterial activities and was the most effective extract, was further fractionated into 8 subfractions with silica gel column chromatography. The subfractions 4 and 5 exhibited an excellent antibacterial activity against Streptococcus iniac KCTC3657.

A Rapid Preparation of Carrier-Free Fluorine-38 for Medical Use

  • Kim, You-Sun;Kim, Jaerok
    • Nuclear Engineering and Technology
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    • v.8 no.1
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    • pp.1-8
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    • 1976
  • For tile rapid production of fluorine-18 for medical use, the up-to-date methods of separation such as the recoil separation, the alumina column chromatography, and the distillation are reviewed. The amount of the residue, the gamma emitting impurity, and the tritium content in the product obtained by each separation method are determined. The product obtained by the nuclear recoil separation or by the alumina column chromatography is inferior to that obtained by the distillation in the purity point of view. Thus, the separation by the distillation is tile most effective especially in the case of using a natural lithium carbonate target. Carrier free fluorine-18 of about 2 mCi can routinely be produced by irradiating 7g of the natural lithium carbonate under the neutron flux of about 1$\times$10$^{13}$ n/$\textrm{cm}^2$/sec for 3 hrs, and subsequent separation by the distillation. The over-all processing time is 35-40n1in.

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Analytical method of the polychlorinated biphenyls in soil using GC/ECD and GC/MS (GC/ECD 및 GC/MS을 이용한 토양 중 PCBs 분석방법 고찰)

  • Kim, Tae-Seung;Shin, Sun-Kyoung;Yoon, Jeong-Ki;Kim, Jong-Ha;Kim, Hyoung Seop;Lee, Jeong Ah
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.91-108
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    • 2007
  • This study was investigated both the Korean official soil test method and the international various methods for PCBs in soil sample. The analytical guideline of PCBs in contaminated soil were proposed based on the official soil test methods by discussing the extraction, column cleanup, instrumental conditions, quantification methods of peak matching and individual isomers. The total 28 soil samples were selected by consideration of PCBs-contamination, land use etc., and then analyzed using gas chromatography/electron capture detection (GC/ECD) and gas chromatography/mass spectrometry(GC/MS). In this study, the PCBs were not detected as peak matching method using GC/ECD, but PCBs detected $0.002{\sim}0.487{\mu}g/kg$ using GC/MS in background concentrations.

Flavonoid Glycosides from Needles of Larix leptolepis(Pinaceae) (일본잎갈나무 잎의 후라보노이드 배당체)

  • Kim, Jin-Kyu;Park, Wan-Geun;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.25 no.2
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    • pp.81-87
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    • 1997
  • 일본잎갈나무잎을 채취하여 아세톤 : 물 (7 : 3, v/v) 의 혼합용액으로 추출한 후 에틸아세테이트용성 화합물과 수용성 화합물로 분리하였으며 Sephadex LH-20으로 충진한 칼럼을 사용하여 화합물을 단리 하였다. 단리 화합물을 확인하기 위하여 셀룰로오스 박층 크로마토그래피(TLC)를 실시한 후 자외선 램프 하에서 관찰하였다. 바닐린 발색제를 분무히여 정색반응을 조사하고 $R_r$ 값을 구하였다. 단리된 화합물들의 구조는 $^1H$-NMR과 $^{13}C$-NMR 스펙트럼을 이용하여 그 구조를 규명하였으며 에틸아세테이트용성 화합물에서는 (+)-catechin, (-)-epicatechin, kaempferol-O-arabinofuranoside와 kaempferol-3-O-arabinopyranoside, 수용성 화합물에서는 apigenin-8-C-rhamnosyl-($1"'{\rightarrow}2"$)-glucoside(2"-O-rhamnosylvitexin)을 단리 하였다.

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Analysis of Characteristics and Dyeing Properties of Gromwell Colorants(Part I) -Components and Characteristics of Gromwell Colorants- (자초색소의 특성분석 및 염색성(제1보) -자초색소의 성분과 특성-)

  • Choi, Hee;Shin, Youn-Sook
    • Journal of the Korean Society of Clothing and Textiles
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    • v.24 no.7
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    • pp.1081-1087
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    • 2000
  • Gromwell colorants were extracted with methanol and dried. Four fractions were obtained by silica gel adsorption column chromatography using step-wise elution method. Relative ratio of four fraction is 1.00:0.07:0.22:0.30(Fl:F2:F3:F4) and gromwell colorants mainly consist of Fl, F3 and F4. IR analysis shows that each fraction has similar structure. Main component of gromwell extracts is acetyl derivative of naphthoquinone, and the rest are isobutyl derivative and isovaleryl derivative etc., in order. Gromwell colorants exhibit relatively good affinity to protein and polyamide fibers, but low affinity to cellulose and regenerated cellulose fibers.

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