• Title/Summary/Keyword: elution yield

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Separation of High Purity Terbium Using Extraction Chromatography (추출 크로마토그래피를 이용한 고순도 테르븀의 분리)

  • Lee, Kwang-Pill;Park, Myoung-Jin;Park, Keung-Shik;Lee, Hueng-Lark;Piao, Zhexiu
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.370-374
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    • 1999
  • Extraction chromatography was used to scarch optimum separation conditions of terbium. Stationary phase was 2-ethylhexyl-2-ethylhexyl phosphonic acid(HEH[EHP])levextrel (-100~+150 mesh), column size was ${\Phi}20{\times}530mm$ and kept constantly temperature at $50^{\circ}C$, adsorption flow rate of $0.2mL/cm^2{\cdot}min$, elution flow rate of $1.0mL/cm^2{\cdot}min$, column diameter to packing height of 1:15. But to search optimum separation conditions of terbium, it changed the eluent acidity, the loading weight of sample. the composition of sample. In conclusion, acidity was 0.6 N HCl, loading weight of sample was about 5% and composition of sample was $Gd_2O_3(20%)+Tb_4O_7(60%)+Dy_2O_3(20%)$. Moreover purity of separated terbium by ICP-AES analysis was 99.98% in yield of 99.99%.

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Efficient Removal of Humic Substances in Preparing DNA Extract from Marine Sediments (해양퇴적물의 핵산추출물에서 humic substances의 효율적인 제거방법)

  • Lee, Jung-Hyun;Shin, Hyun-Hee;Lee, HongKun;Kwon, Kae Kyoung;Ki, Sang-Jin
    • Korean Journal of Microbiology
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    • v.34 no.3
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    • pp.132-136
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    • 1998
  • Molecular analyses of natural microbial communities are often dependent upon the obtainments of pure nucleic acids. The four methods (elution after agarose gel electrophoresis, G-75 microspin columns, hydroxyapatite mi-crospin columns, and polyvinylpolypyrrolidone (PVPP) microspin columns) were compared for the removal of PCR-inhibitory humic substances from the crude DNA extracts of marine sediment samples. The PVPP microspin columns have shown superior removal of humic substances from the crude DNA extract of marine sediment samples, with yield of $4.8{\mu}g/g$ (dry weight of sediment). The purified DNA by this rapid method was pure enough to amplify 1.5 kb fragment corresponding almost full length of 16S rRNA genes.

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Reuse of Eluent by Controlling its Specific Gravity during the Chromatographic Purification of Paclitaxel (크로마토그래피를 이용한 Paclitaxel 정제에서 비중 조절에 의한 Eluent 재사용)

  • Kim, Jin-Hyun
    • KSBB Journal
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    • v.22 no.5
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    • pp.366-369
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    • 2007
  • In this study, the feasibility of reusing the eluent was confirmed by monitoring its specific gravity during the chromatographic purification of paclitaxel from plant cell cultures. The specific gravity of the eluent (methanol/water = 70/30, v/v) was measured prior to its elution through the hydrophobic resin column. The measurement showed a specific gravity of 0.853. The discharged eluent from the column outlet was first evaporated under vacuum pressure. The evaporated eluent was collected and condensed into a liquid eluent again, followed by the HPLC analysis in order to check the presence of any trace of impurity. Even if the specific gravity of the liquid eluent is varied from 0.853 as a result of the evaporation and condensation, the eluent can still be reused after it specific gravity is adjusted by the addition of methanol or water. The reuse of the eluent resulted in the paclitaxel yield of 86% with a purity of 95% which were closely similar to those of before the eluent reuse. These results indicate that the strategy of reusing the eluent on the basis of the specific gravity analysis was successfully implemented in this study.

Simultaneous Determination and Optimization Ultrasound-Assisted Extraction of Poncirin and Naringin in Poncirus trifoliata Rafinesqul (지실의 Poncirin, Naringin의 동시분석법 확립과 초음파 추출법 최적화)

  • Lee, Ah Reum;Jang, Seol;Lee, A Yeong;Choi, Goya;Kim, Hyo Seon;Kim, Ho Kyoung
    • Korean Journal of Medicinal Crop Science
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    • v.22 no.2
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    • pp.147-153
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    • 2014
  • The Ponciri fructus immaturus (Poncirus trifoliata Rafinesque) has been used in oriental medicine for uterine contraction, stomachache, abdominal distension and cardiovascular diseases. Two main compounds, poncirin and naringin were successfully analyzed by high performance liquid chromatography (HPLC) and carried out method validation according to ICH guideline. A successful resolution and retention times were obtained with a $C_{18}$ reversed phase column, at an $1m{\ell}min^{-1}$ flow rate, with a gradient elution of a mixture of methanol, water and acetonitrile. Poncirin and naringin showed good linearity ($R^2$ > 0.999) in relatively wide concentration ranged. The recovery of each compound was 95.81 ~ 101.48% with R.S.D. values less than 1.0%. The application of ultrasound-assisted extraction was shown to be more efficient in extracting poncirin and naringin from Ponciri fructus immaturus. The predicted optimal poncirin and naringin yield were poncirin 2.15%, naringin 1.65% under an extraction temperature of $40^{\circ}C$, an extraction time of 10 min in a solvent of 70% methanol.

Recovery of Isoflavones from Soybean Cooking Water Produced during Soymilk Manufacturing Process (두유 제조 공정에서 생산되는 대두 침지액으로부터 이소플라본의 회수)

  • Choi, Yeon-Bae;Sohn, Heon-Soo
    • Korean Journal of Food Science and Technology
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    • v.29 no.3
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    • pp.522-526
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    • 1997
  • Soy isoflavones could be recovered with adsorption resin column chromatography from soybean cooking water produced during soymilk or tofu manufacturing process. The main isoflavones in the soybean cooking water were genistin and daidzin, and their concentration was $0.083{\pm}0.019$ and $0.11{\pm}0.017\;mM$, respectively. Their aglycones were not detected. pH of soybean cooking water was critical in this chromatographic process and the recovery of isoflavones, both genistin and daidzin, was maximum at pH 4.0. Adsorption of genistin on the resin was stronger than that of daidzin. Elution rate and height/diameter ratio also affected the recovery yield. Under the optimal conditions, about 85% of genistin and 70% of daidzin could be isolated from soybean cooking water. Soy saponins were also recovered with isoflavones.

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Graft Copolymerization to Proteins (II). Separation and Purification of Sericin, and Its Graft Copolymerization with Acrylonitrile (단백질에 대한 그라프트 공중합 (제2보). 세리신의 분리, 정제 및 아크릴로니트릴의 그라프트 공중합)

  • Iwhan Cho;Kwang-Kun Kim
    • Journal of the Korean Chemical Society
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    • v.20 no.4
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    • pp.309-315
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    • 1976
  • An efficient separation method and the utilization of sericin are searched. Sericin was extracted with hot water from cocoons under atmospheric pressure. The separated sericin was gel-filtrated with Sephadex G-75 and G-150 at room temperature and at $70^{\circ}C$. The results indicated that sericin is consisted of only one fraction in elution diagram. In the graft copolymerization of acrylonitrile to sericin ceric ammonium nitrate was chosen as an initiatior. A maximum yield was obtained at certain concentration of the initiator confirming our previous experiments. Viscosity measurement of alkali-hydrolyzed graft copolymers indicated that the polyacrylonitrile graft had the molecular weight in the range of 7,000.

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Separation of Goid, Palladium and Platinum in Chromite by Anion Exchange Chromatography for Inductively Coupled Plasma Atomic Emission Spectrometric Analysis

  • Choe, Gwang Sun;Lee, Chang Hyeon;Park, Yeong Jae;Jo, Gi Su;Kim, Won Ho
    • Bulletin of the Korean Chemical Society
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    • v.22 no.8
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    • pp.801-806
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    • 2001
  • A study has been carried out on the separation of gold, iridium, palladium, rhodium, ruthenium and platinum in chromite samples and their quantitative determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution condition of the minerals by fusion with sodium peroxide was optimized and chromatographic elution behaviour of the rare metals was investigated by anion exchange chromatography. Spectral interference of chromium, a matrix of the minerals, was investigated on determination of gold. Chromium interfered on determination of gold at the concentration of 500 mg/L and higher. Gold plus trace amounts of iridium, palladium, rhodium and ruthenium, which must be preconcentrated before ICP-AES was separated by anion exchange chromatography after reducing Cr(Ⅵ) to Cr(III) by H2O2. AuCl4- retained on the resin column was selectively eluted with acetone- HNO3-H2O as an eluent. In addition, iridium, palladium, rhodium and ruthenium remaining on the resin column were eluted as a group with concentrated HCl. However, platinum was eluted with concentrated HNO3. The recovery yield of gold with acetone-HNO3-H2O was 100.7 ${\pm}2.0%$, and the yields of palladium and platinum with concentrated HCl and HNO3 were 96.1 ${\pm}1.8%$ and 96.6 ${\pm}1.3%$, respectively. The contents of gold and platinum in a Mongolian chromite sample were 32.6 ${\pm}$ 2.2 ${\mu}g$/g and 1.6 $\pm$ 0.14 ${\mu}g$/g, respectively. Palladium was not detected.

HPLC/UV Quantification of (+)-Catechin in Filipendula glaberrima from Different Regions and Flowering Stages (터리풀의 채집장소 및 채집시기에 따른 카테킨 함량 HPLC/UV 분석)

  • Lee, Hak-Dong;Lee, Yunji;Kim, Hoon;Kim, Hangeun;Park, Chun-Gun;Lee, Sanghyun
    • Korean Journal of Pharmacognosy
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    • v.51 no.4
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    • pp.291-296
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    • 2020
  • Filipendula glaberrima (FG) is a plant endemic to South Korea. It is economically important as a food source and used as a medicine in treating ailments. Filipendula flowers are characterized by the presence of several polyphenolic constituents. The aim of this study is to determine the content of (+)-catechin in Filipendula glaberrima collected from different regions at different flowering stages. High-performance liquid chromatography with a gradient elution system (0.5% acetic acid in water : acetonitrile = 95 : 5 to 0 : 100 for 35 min) was used. A reverse-phase INNO column with UV detection at 278 nm was employed. The results revealed that F. glaberrima from Mt. Odae has the highest (+)-catechin content (10.600 mg/g). Furthermore, its content was the lowest in samples collected during the pre-flowering period and the highest at the early-flowering stage. This study provides a basis in establishing the optimal period and the best region for collecting F. glaberrima with maximized (+)-catechin yield.

Toxin Produced by Pathogenic Vibrios Isolated from Sea Food (수산물에서 분리된 병원성 비브리오균의 용혈성독소)

  • CHANG Dong-Suck;SHINODA Sumio
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.27 no.2
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    • pp.107-113
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    • 1994
  • Among the currently recognized pathogenic vibrios, V. vulnificus and V. cholerae non O1 are the most serious bacteria from the point of view of sea food hygiene in Korea. In this paper, the authors compared the hemolytic activities of the crude hemolysin produced by V. vulnificus and V. cholerae non O1 isolated from shellfish collected in Chungmoo, Korea. The authors also attempted to improve the purification method of V. vulnificus hemolysin(VVH) and tried to make antiserum with the purified hemolysin. VVH was produced in abundance in heart infusion broth containing $2\%$ NaCl in a shaking cultivation process(140rpm) at $37^{\circ}C$ for 15 hours. While hemolysin production patterns of V. cholerae non O1 were quite different by the strain during the culture times compared with the V. vulnificus. Hemolytic activity of the VVH on sheep erythrocytes was stronger than those of rabbit, but hemolytic activities of the hemolysin produced by V. cholerae non O1 on rabbit erythrocytes were as much as twice as strong as on those of sheep and horse. VVH was purified by two steps of hydrophobic column chromatography on Phenyl-Sepharose HP with Fast Protein Liquid Chromatography(FPLC). Purification fold and yield of VVH was much improved by changing the elution buffer's pH from 6.0 to 9.8 and adding $1\%$ CHAPS(a zwitter ionic detergent) and $50\%$ ethylene glycol to the 10mM glycine buffer during the repeated hydrophobic column chromatography. Homogeneity of the purified hemolysin was shown by polyacrylamide gel electrophoresis. According to the five times repeated purification results, the specific activity was increased 27500 times and the yield was improved by $23.4\%$ on average. About $250{\mu}g$ of purified hemolysin was harvested from the 2400ml of culture supernatant of V. vulnificus. Molecular weight of VVH was estimated to be 50KDa by the SDS-PAGE and the neutralization scores of the obtained antiserum acting against VVH were $2000{\sim}8500$.

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Evaluation on Extraction Conditions and HPLC Analysis Method for Bioactive Compounds of Astragali Radix (황기의 추출조건 및 유효성분의 HPLC 분석법 평가)

  • Kim, Geum Soog;Lee, Dae Young;Lee, Seung Eun;Noh, Hyung Jun;Choi, Je Hun;Park, Chun Geun;Choi, Soo Im;Hong, Seung Jae;Kim, Seung Yu
    • Korean Journal of Medicinal Crop Science
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    • v.21 no.6
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    • pp.486-492
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    • 2013
  • This study has been conducted to establish the optimal extraction process and HPLC analysis method for the determination of marker compounds as a part of the materials standardization for the development of health functional food materials from Astragali radix. Five extraction conditions including the shaking extraction at room temperature and the reflux extraction at $85^{\circ}C$ with 30%, 50% and 95% ethanol were evaluated. Reflux extraction with 50% ethanol showed the highest extraction yield as $27.27{\pm}2.27%$, while the extraction under reflux with 95% ethanol showed significantly the lowest yield of $10.55{\pm}0.24%$. The quantitative determination methods of calycosin-7-O-${\beta}$-D-glucoside and calycosin as marker compounds of Astragali radix extracts were optimized by HPLC analysis using a Thermo Hypersil column ($4.6{\times}250mm$, $5{\mu}m$) with the gradient elution of water and acetonitrile as the mobile phase at the flow rate of $0.8mLmin^{-1}$ and a detection wavelength of 230nm. The HPLC/UV method was applied successfully to the quantification of two marker compounds in Astragali radix extracts after validation of the method with the linearity, accuracy and precision. The contents of calycosin-7-O-${\beta}$-D-glucoside and calycosin in 50% ethanol extracts by reflux extraction were significantly higher as $1,700.3{\pm}30.4$ and $443.6{\pm}8.4{\mu}g-1$, respectively, comparing with those in other extracts. The results indicate that the reflux extraction with 50% ethanol at $85^{\circ}C$ is optimal for the extraction of Astragali radix, and the established HPLC method are very useful for the evaluation of marker compounds in Astragali radix extracts to develop the health functional material from Astragali radix.