• Title/Summary/Keyword: liquid flow

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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 Separation of Lysozyme from Egg White by Ion Exchange Column Chromatography (이온교환 칼럼 크로마토그래피를 이용한 난백에서 Lysozyme의 연속추출)

  • Park, Seong-Joon;Kim, Hyeon-Seok;Kim, Hyean-Wee;Ahn, Tae-Hoe;Park, Ki-Moon;Choi, Chun-Un
    • Korean Journal of Food Science and Technology
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    • v.22 no.6
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    • pp.711-715
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    • 1990
  • Continuous column chromatographic separation of lysozyme from egg white was investigated. A weak acid type cation exchange resin, Duolite C-464, was used because of high lysozyme recovery and ease of column operation in this experiment. The resin was equilibrated at $pH\;7.9{\pm}0.1$ in Na+form. Continuous lysozyme separation was processed by repeating cycles(one cycle : resin equilibration, flow egg white, rinse, lysozyme elution) in automated preparative Liquid Chromatography(LC) system(column size ; i.d. 50 mm, resin bed volumn ; 1020 ml). At comparison of UV levels in rinse end point and elution end point of every cycle, the UV levels of rinse end point are maintained below 30% for 19 cycles and that of elution end point are also maintained below 30% for 17 cycles, stably, but was increased above 50% after 18 cycle. That indicated the eluting ability of lysozyme was reduced conspicuously after 18 cycle in continuous cycling process. The recovery of lysozyme was maintained above 90% from one to 17 cycle, but was decreased to 72% and 65% in 18 cycle and 19 cycle, respectively.

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A Study on Capillary Gas-Liquid Chromatographic Determination of Diosgenin in Costus Speciosus (모세관 기체-액체 크로마토그래피에 의한 Costus Speciosus 중 Diosgenin의 정량에 관한 연구)

  • Taek Jae Kim;Cha Kee Surk;Kim Young Sang
    • Journal of the Korean Chemical Society
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    • v.30 no.4
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    • pp.369-376
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    • 1986
  • Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.

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Estimation of Impurities from Commercially Available Glycyrrhizin Standards by the HPLC/ESI-MS (HPLC/ESI-MS에 의한 글리시리진 표준품의 불순물 추정)

  • Myung, Seung-Woon;Min, Hye-Ki;Kim, Myungsoo;Kim, Young Lim;Park, Seong-Soo;Cho, Jung Hee;Lee, Jong-Chul;Cho, Hyun-Woo;Kim, Taek-Jae
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.504-510
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    • 2000
  • The impurity profiles from the raw materials of glycyrrhizin were performed by the high performance liquid chromatography (HPLC)/electrospray ionization (ESI)- mass spectrometry (MS). For the HPLC experiment, a $C_{18}$($3.9{\times}300mm$, $10{\mu}m$) column was used and the mobile phase was acetic acid/$H_2O$ (1:10):acetonitrile=3:2 with a flow rate of 0.8 ml/min. The effluent was splitted into the ratio of 50:1 and went into the ESI-MS. Three to six impurities were found and informed of the identification of the structure of the impurities by ESI-MS. And the structures of impurities were suggested to a hydroxy-glycyrrhizin which is added with hydroxy group (-OH) in the glycyrrhetic acid moiety and a reduced-glycyrrhizin which the position of 12 of the glycyrrhetic acid moiety is reduced. The purities of the standard materials were about 90%.

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Development of Numerical Method for Large Deformation of Soil Using Particle Method (입자법을 이용한 토사의 대변형 해석법 개발)

  • Park, Sung-Sik;Lee, Do-Hyun;Kwon, Min-Ho
    • Journal of the Korean Geotechnical Society
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    • v.29 no.12
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    • pp.35-44
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    • 2013
  • In this study, a particle method without using grid was applied for analysing large deformation problems in soil flows instead of using ordinary finite element or finite difference methods. In the particle method, a continuum equation was discretized by various particle interaction models corresponding to differential operators such as gradient, divergence, and Laplacian. Soil behavior changes from solid to liquid state with increasing water content or external load. The Mohr-Coulomb failure criterion was incorporated into the particle method to analyze such three-dimensional soil behavior. The yielding and hardening behavior of soil before failure was analyzed by treating soil as a viscous liquid. First of all, a sand column test without confining pressure and strength was carried out and then a self-standing clay column test with cohesion was carried out. Large deformation from such column tests due to soil yielding or failure was used for verifying the developed particle method. The developed particle method was able to simulate the three-dimensional plastic deformation of soils due to yielding before failure and calculate the variation of normal and shear stresses both in sand and clay columns.

A Study of Heat Transfer during Freezing Process of Water in a Vertical Cylinder - Comparison of thermal storage performance on the working fluid direction - (수직원통형 축열조내 물의 응고과정시 열전달에 관한 실험적연구 - 작동유체의 유동방향에 따른 열저장성능 비교 -)

  • Heo, K.;Kim, Y.K.;Kim, Y.J.;Kim, J.K.;Yim, C.S.
    • Solar Energy
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    • v.15 no.2
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    • pp.77-90
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    • 1995
  • An effective heat transfer during freezing process was proposed in the vertical cylinder to improve the effectiveness of the heat storage. Vertical cylinder was filled with pure water in order to investigate ice-shape, temperature distribution of the liquid, temperature distribution of the cylinder tube wall, total heat storage per unit mass in the test section under the two experimental conditions; inlet temperature of working fluid is constant($-10^{\circ}C$) and inlet direction of working fluid is either upward flow or downward. Both the mean temperature of the liquid and temperature difference of cylinder tube wall in the upward were lower than those in the downward. In case that the initial temperature of water was $7^{\circ}C$ and $4^{\circ}C$, the shape of ice layer in the upward was more uniform than that in the downward. In case of $1^{\circ}C$, the shape of ice layer is formed by inlet direction of working fluid. Finally, time-varying total heat energy stored in the water in the upward was higher than that in the downward.

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The Numerical Study on Effect of the Droplet Sizes on Internal Mass Transfer in the Spray Type Scrubber (분무형 스크러버에 내에서 액적크기에 따른 물질전달에 관한 전산해석적 연구)

  • Lee, Chanhyun;Chang, Hyuksang
    • Clean Technology
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    • v.25 no.1
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    • pp.19-32
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    • 2019
  • As regional air pollution gets worse by the sulfur oxides emitted from various types of vessels passing through the many countries, the International Maritime Organization establishes the emission control areas and regulates sulfur dioxide in those areas. In order to satisfy these regional regulations, the fuel selection method and the exhaust gas post-treatment device are applied to the ships. Due to the economic reasons, the post-treatment method of exhaust gas for reducing the amount of sulfur oxides discharged is mainly preferred. The scrubber which is dominantly used in the ships are the spray type system where the sprayed liquid drops used for capturing the soluble sulfur dioxides in the exhaust gas. The performance of the spray type system depends on the size distribution of the sprayed droplets. In order to evaluate this performance, we designed counterflow type scrubber and cyclone scrubber and evaluated the desulfurization efficiency and the amount of droplet evaporation according to the size of each droplet by using computational fluid dynamics. The Eulerian-Eulerian analysis method was used because the scrubber had a gas-liquid two-phase flow inside the scrubber. When the diameter of the droplet was $100{\mu}m$, $300{\mu}m$, $500{\mu}m$ and $700{\mu}m$. As a result, both of scrubbers showed high desulfurization efficiency and low evaporation amount at $500{\mu}m$ and $700{\mu}m$.

Analytical Method Development of (-)-Epicatechin gallate in Penthorum chinense Pursh Extract using HPLC (HPLC를 이용한 낙지다리 추출물의 (-)-­Epicatechin gallate 분석법 개발)

  • Kwon, Jin Gwan;Jung, Yeon Woo;Seo, Changon;Hong, Seong Su;Choi, Chun Whan;Lee, Ji Eun;Shin, Hyun Tak;Jung, Su Young;Kim, Jin Kyu
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.45 no.1
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    • pp.87-93
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    • 2019
  • This study attempted to eatablish a High Performance Liquid Chromatography (HPLC) analysis method for the determination of (-)-epicatechin gallate as a part of the quality control for the development of functional cosmetic materials from Penthorum chinense Pursh. HPLC was performed on a Unison $US-C_{18}$ column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and methyl alcohol at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analyte was detected at 280 nm. The HPLC method was performed in accordance with the International Conference on Harmonization (ICH) guideline (version 4, 2005) of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation were 0.11 and 0.33 mg/mL, respectively. Calibration curves showed good linearity ($r^2$ > 0.9999), and the precision of analysis was satisfied (less than 0.6%). Recoveries of quantified compounds ranged from 99.51 to 101.92%. This result indicates that the established HPLC method is very useful for the determination of marker compound in P. chinense Pursh extracts.

Development and validation of an LC-MS/MS method for the simultaneous analysis of 26 anti-diabetic drugs in adulterated dietary supplements and its application to a forensic sample

  • Kim, Nam Sook;Yoo, Geum Joo;Kim, Kyu Yeon;Lee, Ji Hyun;Park, Sung-Kwan;Baek, Sun Young;Kang, Hoil
    • Analytical Science and Technology
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    • v.32 no.2
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    • pp.35-47
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    • 2019
  • In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

Pogo Suppressor Design of a Space Launch Vehicle using Multiple-Objective Optimization Approach (다목적함수 최적화 기법을 이용한 우주발사체의 포고억제기 설계)

  • Yoon, NamKyung;Yoo, JeongUk;Park, KookJin;Shin, SangJoon
    • Journal of the Korean Society of Propulsion Engineers
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    • v.25 no.1
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    • pp.1-11
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    • 2021
  • POGO is a dynamic axial instability phenomenon that occurs in liquid-propelled rockets. As the natural frequencies of the fuselage and those of the propellant supply system become closer, the entire system will become unstable. To predict POGO, the propellant (oxidant and fuel) tank in the first stage is modeled as a shell element, and the remaining components, the engine and the upper part, are modeled as mass-spring, and structural analysis is performed. The transmission line model is used to predict the pressure and flow perturbation of the propellant supply system. In this paper, the closed-loop transfer function is constructed by integrating the fuselage structure and fluid modeling as described above. The pogo suppressor consists of a branch pipe and an accumulator that absorbs pressure fluctuations in a passive manner and is located in the middle of the propellant supply system. The design parameters for its design optimization to suppress the decay phenomenon are set as the diameter, length of the branch pipe, and accumulator. Multiple-objective function optimization is performed by setting the energy minimization of the closed loop transfer function in terms of to the mass of the pogo suppressor and that of the propellant as the objective function.