• Title/Summary/Keyword: two-phase solvent system

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A Study of the Retention Mechanism of the Monosubstituted Benzenes in Reversed-Phase Liquid Chromatography (Ⅰ). The Elution Behavior of the Monosubstituted Benzenes (역상 액체크로마토그래피에서 벤젠 일치환체들의 머무름 메카니즘에 관한 연구 (Ⅰ). 벤젠 일치환체들의 용리거동)

  • Dai Woon Lee;Yong Wook Choi;Hyun Joo Kim;Yong Soon Chung
    • Journal of the Korean Chemical Society
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    • v.31 no.1
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    • pp.55-63
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    • 1987
  • The systematic investigation of the retention behaviors of 18 monosubstituted benzenes in reversed-phase liquid chromatography(RPLC) was studied in order to predict the separation possibility of their mixtures and study the contribution of substituent group to the retentions of solutes. The columns and mobile phases employed in this study were $\mu$ -Bondapak $C_{18}$, $\mu$-Bondapak phenyl columns and methanol/water, acetonitrile/water, and THF/water, respectively. The polar substituents such as phenol, aniline, acetophenone and benzonitrile have smaller capacity factor(k') values than benzene, while nonpolar ones such as alkylbenzenes and halobenzenes show larger k' value. The capacity factors of all solutes increased on both C18 bonded and phenyl bonded phases as the organic solvent content of three organic solvent-water mixtures decreased. The absolute differences in capacity factor(${\Delta}k$') between substituent and benzene were graphically shown for the prediction of the separation of the mixture and interpretation of the elution behavior of substituent. In addition, the selectivity of solvent system for the separation of the mixture was investigated in both two columns and three mobile phases.

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Phase Behavior of Poly(ethylene-co-vinyl alcohol)-Solvent System at High Pressure (고압에서 폴리(에틸렌/비닐 알코올) 공중합체-용매계의 상거동에 관한 연구)

  • Byun, Hun-Soo;Kim, Chong-Bae
    • Applied Chemistry for Engineering
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    • v.9 no.3
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    • pp.424-429
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    • 1998
  • Cloud-point data at $230^{\circ}C$ and 1,800 bar are presented for two poly(ethylene-co-vinyl alcohol)(PEVA) copolymers[9.9mol% and 17.8mol% vinyl alcohol(VA)] in ethylene, propane, propylene, n-butane, 1-butene, dimethyl ether(DME), and chlorodifluromethane(CDFM). The static type experimental apparatus with a view cell has been used for the experiment at the high pressure and temperature. The pressure-temperature (P-T) loops of PEVA(9.9mol% VA) copolymer-DME mixtures are presented at copolymer concentrations of 1.4wt% to 20.0wt%. Also, we presented the phase behavior of PEVA(17.8mol% VA) copolymer-DME system at copolymer concentration of 1.9wt% to 6.8wt%. The cloud-point curves for the PEVA copolymers in dimethyl ether showed single phase above 480 bar as a result of the hydrogen bonding between the vinyl alcohol unit and dimethyl ether. The pressure-concentration(P-x) isotherm loops of PEVA(9.9mol% and 17.8mol% VA)-DME system are obtained. The cloud-point curves for PEVA(9.9mol% and 17.8 mol% VA) copolymers andthe ethylene, propane, propylene, n-butane, 1-butene, and CDFM all show negative slopes of phase behavior and are located at pressures below 1,800 bar. For PEVA copolymer-DME system(9.9mol% VA), cloud-point curves show positive slopes that decrease in pressures with decrease in temperature in the temperature range of $80^{\circ}C$ to $160^{\circ}C$.

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Isolation of Berberine from the Rhizome of $Coptis$ $chinensis$ by Centrifugal Partition Chromatography (향류분배 크로마토그라피법에 의한 황련($Coptis$ $chinensis$) 뿌리로 부터 Berberine의 분리)

  • Kim, Jung-Bae
    • The Korean Journal of Food And Nutrition
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    • v.24 no.4
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    • pp.617-621
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    • 2011
  • $Coptis$ $chinensis$ Franch rhizome is one of the important traditional Korea medicines with anti-inflammatory, anti-bacterial, anti-hypertensive and anti-cancer properties. The methanol extract of rhizome from the $Coptis$ $chinensis$ rhizome was purified by using preparative centrifugal partition chromatography (CPC) and HPLC method. The optimum two-phase CPC solvent system was composed of n-butanol:acetic acid:water at a ratio of 4:1:5. Berberine (16.8 mg) was successfully isolated by CPC and HPLC. The chemical structure of the compound was identified by (1 H)$^1H$, $^{13}C$-NMR and ESI-MS spectral data analysis.

Isolation and Purification of Antibacterial Components in Cortex Phellodendri (황백나무로부터 항균성분의 분리 및 정제)

  • Kim, Jung-Bae;Shin, Woon-Seob;Kwon, Young-In;Bang, Byung-Ho
    • The Korean Journal of Food And Nutrition
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    • v.26 no.3
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    • pp.547-552
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    • 2013
  • Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections and infections of the body surface. In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out to separate antibacterial compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 $m{\ell}/min$ in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. Palmatine weas identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

Isolation and Purification of Berberine in Cortex Phellodendri by Centrifugal Partition Chromatography (Centrifugal Partition Chromatography에 의한 황백으로부터 Berberine의 분리 및 정제)

  • Kim, Jung-Bae;Bang, Byung-Ho
    • The Korean Journal of Food And Nutrition
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    • v.27 no.3
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    • pp.532-537
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    • 2014
  • Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections, and infections of the body surface. Many analytical methods have been used to study oriental herbal medicines, such as thin-layer chromatography, column liquid chromatography, and high performance liquid chromatography (HPLC). In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out in order to separate pure compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 mL/min in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. The $^1H$ NMR spectrum revealed that the resonances at ${\delta}$ 4.10 and 4.20 ppm corresponded to three protons ($-OCH_3$), whereas those at ${\delta}$ 6.10 ppm corresponded to two protons ($-OCH_2O-$). Further, two aromatic protons (H-11 and H-12) conveys a doublet-doublet pattern. The H-11 doublet and H-12 doublet appear at ${\delta}$ 7.98 and 8.11, respectively. The $^{13}C$ NMR. spectrum showed a tetrasubstituted with a methylenedioxy group at C2 and C3, and two methoxy groups at C9 and C10. The chemical structure of the berberine was identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

Continuous Process for the Etching, Rinsing and Drying of MEMS Using Supercritical Carbon Dioxide (초임계 이산화탄소를 이용한 미세전자기계시스템의 식각, 세정, 건조 연속 공정)

  • Min, Seon Ki;Han, Gap Su;You, Seong-sik
    • Korean Chemical Engineering Research
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    • v.53 no.5
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    • pp.557-564
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    • 2015
  • The previous etching, rinsing and drying processes of wafers for MEMS (microelectromechanical system) using SC-$CO_2$ (supercritical-$CO_2$) consists of two steps. Firstly, MEMS-wafers are etched by organic solvent in a separate etching equipment from the high pressure dryer and then moved to the high pressure dryer to rinse and dry them using SC-$CO_2$. We found that the previous two step process could be applied to etch and dry wafers for MEMS but could not confirm the reproducibility through several experiments. We thought the cause of that was the stiction of structures occurring due to vaporization of the etching solvent during moving MEMS wafer to high pressure dryer after etching it outside. In order to improve the structure stiction problem, we designed a continuous process for etching, rinsing and drying MEMS-wafers using SC-$CO_2$ without moving them. And we also wanted to know relations of states of carbon dioxide (gas, liquid, supercritical fluid) to the structure stiction problem. In the case of using gas carbon dioxide (3 MPa, $25^{\circ}C$) as an etching solvent, we could obtain well-treated MEMS-wafers without stiction and confirm the reproducibility of experimental results. The quantity of rinsing solvent used could be also reduced compared with the previous technology. In the case of using liquid carbon dioxide (3 MPa, $5^{\circ}C$, we could not obtain well-treated MEMS-wafers without stiction due to the phase separation of between liquid carbon dioxide and etching co-solvent(acetone). In the case of using SC-$CO_2$ (7.5 Mpa, $40^{\circ}C$), we had as good results as those of the case using gas-$CO_2$. Besides the processing time was shortened compared with that of the case of using gas-$CO_2$.

Lupin Seed for Human Consumption (루우핀 콩의 식품이용)

  • Lee, Cherl-Ho
    • Korean Journal of Food Science and Technology
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    • v.18 no.5
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    • pp.398-405
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    • 1986
  • The food quality of lupin seed, i.e. soaking, cooking, sprout growing and mold growing for fermentation, was investigated by using the seed of Lupinus angustifolius harvested in Western Australia. A method to produce lupin seed protein concentrate (LPC) was developed, and the wage of LPC in Korean food system was investigated. The water soaking rate of lupin seed was faster than that of soybean, but the cooking rate of lupin seed was much slower compared to soybean. The thermal softening time, $D_{100}$, was 345 min for lupin seed and 84 min for soybean. A two-phase solvent extraction system consisting of haxane-alcohol-water could effectively remove the residual bitter taste, lipid and yellow pigments of lupin seed flour, and the resulting LPC contained over 50% protein and had bland flavor and milky white color. Treatment of LPC with carbohydrate decomposing enzymes resulted in a product of more soluble and higher concentration of protein. Methods to produce lupin seed vegetable milk and lactic beverages from LPC products were discussed.

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Thermal Degradation Kinetics of Tocopherols during Heating without Oxygen (무산소 가열시 토코페롤의 열분해 키네틱스)

  • Chung, Hae-Young
    • The Korean Journal of Food And Nutrition
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    • v.20 no.2
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    • pp.120-124
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    • 2007
  • The thermal degradation kinetics of alpha-, gamma- and delta-tocopherols was studied during heating at 100, 150 200 and 250$^{\circ}C$ for 5, 15, 30 and 60 min in the absence of oxygen. The tocopherols were separated by HPLC using a reversed phase ${\mu}$-Bondapak C$_{18}$-column with two kinds of elution solvent system in a gradient mode. The kinetics for degradation of ${\alpha}$-, ${\gamma}$- and ${\delta}$-tocopherols was analyzed as a function of temperatures and times. The degradation of tocopherols was described by the first-order kinetics in the absence of oxygen. The rate of tocopherols degradation was dependent on heating temperatures. The degradation rate constants for ${\alpha}$-, ${\gamma}$ and ${\delta}$-tocopherols showed an increasing trend as the heating temperature increased. The magnitude order of the experimental activation energy was ${\delta}$->${\gamma}$->${\alpha}$-tocopherol.

Isolation of Eckol from Ecklonia cava via Centrifugal Partition Chromatography (CPC) and Characterization of it's Anti-inflammatory Activity (고속원심분배 크로마토그래피를 이용한 감태(Ecklonia cava)로부터 Eckol의 분리 및 항염증 활성)

  • Kim, Yoon Taek;Lee, Ji-Hyeok;Ko, Ju-Young;Oh, Jae-Young;Lee, Won-U;Sok, Chang Hyun;Hong, Jin Tae;Jeon, You-Jin
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.48 no.3
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    • pp.301-307
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    • 2015
  • Phlorotannins and marine algal polyphenols, including dieckol, 6,6-bieckol, phloroglucinol, phlorofucofuroeckol-A, and eckol, were isolated from brown seaweeds. These compounds have beneficial bioactivities, and Ecklonia cava has become widely used for the extraction and isolation of phlorotannins. Eckol, in particular, has been to shown to have antioxidant, anti-inflammatory, anticoagulatory, and photoprotective properties. However, due to its low abundance in weaweed, the isolation and purification of eckol are difficult. Its limited availability renders the isolation and purification of eckol labor-intensive processes. Centrifugal partition chromatography (CPC) is an efficient technique for the isolation and purification of eckol. In this study, eckol was isolated from the ethyl acetate fraction of the 70% ethanol extract of E. cava using CPC with a two-phase solvent system of a n-hexane:EtOAc:methanol:water (2:8:3:7, v/v) solution. The purity and anti-inflammatory activity of the isolated eckol were verified by high-performance liquid chromatography and by assaying lipopolysaccharide-induced inflammatory responses in an immortalized murine BV2 microglial cell line, respectively. In conclusion, CPC is a useful technique for simple and efficient isolation of eckol from E. cava.

Evaluation of A Removal Process for the Residual Uranium from the Simulated Radwaste Solution by Solvent Extraction with TBP (TBP 용매추출에 의한 잔존 우라늄 제거공정 평가)

  • Lee, Eil-Hee;Kim, Kwang-Wook;Lim, Jae-Gwan;Kwon, Seon-Gil;Yoo, Jae-Hyung
    • Applied Chemistry for Engineering
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    • v.9 no.2
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    • pp.232-237
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    • 1998
  • This study was carried out to find the optimal operating conditions for separation of residual uranium from the simulated radwaste solution containing 19 elements, and to evaluate the validity of the process. The selected process was based on the solvent extraction with TBP(tributyl phosphate). As an extractor, two miniature mixer-settlers with a total of 18 stages were used. Extraction yield of U, Np and Tc was about 99.2%. 32.1%, and 99.9%, respectively. The other elements were coextracted in the range of 1~4%. Extraction yield of U exceeded those of the previous work performed with batch system, which resulted in the low extractability of U (about 80%) according to the coexisting element such as Nd and Fe. It was due to the characteristics of multi-stage extractor. On the other hand, low extractability of Np was caused by various oxidation states in the nitric acid medium. In the case of Tc, its high extractability may be attributed to the complex formation with Zr and U, which is not well proved yet. All elements extracted with TBP were stripped into aqueous phase more than 99% by 0.01M $HNO_3$. From the results, this process has no problem with respect to in the same step was required, because Np was distributed in the raffinate and U product, respectively.

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