• Title/Summary/Keyword: solid-phase method

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Rapid Gas Chromatographic Profiling and Screening of Acidic Non-Steroidal Antiinflammatory Drugs in Biological Samples

  • Kim, Kyoung-Rae;Shin, You-Jin;Shim, Won-Hee;Myung, Seoung-Won
    • Archives of Pharmacal Research
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    • v.17 no.3
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    • pp.175-181
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    • 1994
  • The solid-phase extraction (SPF) with subsequent tert-butyldimethylsilyl (TBDMS) derivatization was investigated for the rapid profiling and screening of various carboxylated non-steroidal antiinflammatory drugs (NSAIDs) simultaneously in biological fluid samples. Compared to the conventional SPF in adsorption mode using Chromosorb 102, Chromosorb 107, Carbopak B and Thermosorb, the SPF in partition mode using Chromosorb P as the adsorbent, and ethyl acetate/methylene chloride as the eluting solvents provided hightest overall recovenies of the NSAIDs from aqueous solutions with good precision. The solid-phase extracted NASIDs were silylated with N-methyl-N-(tert-butyldimethylsily)trifuoroacetamide to TBDMS derivatives and directly analyzed by capillary gas chromatography and gs chromatography-mass spectrometry. The usefulness of the present method was examined for the profilling and screening of saliva, serum and urine samples for various NSAIDs simultaneously.

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Thermoviscoelastic orthotropic solid cylinder with variable thermal conductivity subjected to temperature pulse heating

  • Abouelregal, A.E.;Zenkour, A.M.
    • Earthquakes and Structures
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    • v.13 no.2
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    • pp.201-209
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    • 2017
  • This work aims to analyze the thermo-viscoelastic interaction in an orthotropic solid cylinder. The medium is considered to be variable thermal conductivity and subjected to temperature pulse. Analytical solution based on dual-phase-lags model with Voigt-type for behavior of viscoelastic material has been effectively proposed. All variables are deduced using method of Laplace transforms. Numerical results for different distribution fields, such as temperature, displacement and stress components are graphically presented. Results are discussed to illustrate the effect of variability thermal conductivity parameter as well as phase-lags and viscoelasticity on the field quantities. Results are obtained when the viscosity is ignored with and without considering variability of thermal conductivity. A comparison study is made and all results are investigated.

Chiral Separation of Salbutamol Enantiomers in Human Plasma

  • Seo, Joung-Min;Kim, Kyeong-Ho
    • Archives of Pharmacal Research
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    • v.17 no.4
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    • pp.244-248
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    • 1994
  • A stereoselective and sensitive high performance liquid chromatography using fluoresecence deterctor was examined for the determination of R(-) and S(+)-salbutamol in human plasma. Solid phase extraction method using silica as sorbent was used to extract salbutamol racemates from the plasma matrices. After fractionation and freeze-drying of the eluates containing salbutamol racemates, they were separated and quantified on a chirla stationary column. The detection limit of each enantiomer was 2 ng/ml in human plasma (S/N=3).

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Comparison of Different Solid-Phase Extraction Methods for the Analysis of Heterocyclic Amines from Pan-Fried Pork Meat (가열 조리된 돼지고기의 Heterocyclic Amines 분석을 위한 Solid-phase 추출 방법의 비교)

  • Lee, Jae-Hwan;Back, Yu-Mi;Lee, Kwang-Geun;Shin, Han-Seung
    • Food Science of Animal Resources
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    • v.28 no.5
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    • pp.637-644
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    • 2008
  • Four different extraction and purification methods were evaluated to determine the heterocyclic amines (HCAs) in fried pork patties. Pork patties were cooked in the teflon-coated electric frying pan at $230^{\circ}C$ for 8 min per side. HCAs in the fried pork patties were extracted and purified using four different solid-phase extraction (SPE) methods and quantitated by LC-MS (API-ESI). Recovery of four different extraction and purification methods was evaluated by comparing the HCAs amounts quantified by the standard addition method. Validation of extraction and purification methods for fried pork patties was determined to establish accurate sample preparation. The recoveries of HCAs from different SPE methods were calculated. The recovery yields were 15.7-68.7% (Polar amine group) and 25.0-74.7% (less-polar amine group) in method A. Method D provided recovery yields ranging from 14.1% to 68.7% in polar amine groups and from 3.0% to 72.3% in less-polar amine groups, respectively. Modified procedures of Method A and D were the most suitable extraction and purification method for HCAs analysis from fried pork patties.

Effects of Density Change and Cooling Rate on Heat Transfer and Thermal Stress During Vertical Solidification Process (수직응고 시스템에서 밀도차와 냉각률이 열전달 및 열응력에 미치는 영향)

  • 황기영;이진호
    • Transactions of the Korean Society of Mechanical Engineers
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    • v.19 no.4
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    • pp.1095-1101
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    • 1995
  • Numerical analysis of vertical solidification process allowing solid-liquid density change is performed by a hybrid method between a winite volume method (FVM) and a finite element method (FEM). The investigation focuses on the influence of solid-liquid density change and cooling rates on the motion of solid-liquid interface, solidified mass fraction, temperatures and thermal stresses in the solid region. Due to the density change of pure aluminium, solid-liquid interface moves more slowly but the solidified mass fraction is larger. The cooling rate of the wall is shown to have a significant influence on the phase change heat transfer and thermal stresses, while the density change has a small influence on the motion of the interface, solidified mass fraction, temperature distributions and thermal stresses. As the cooling rate increases, the thermal stresses become higher at the early stage of a solidification process, but it has small influence on the final stresses as the steady state is reached.

On-line SPE-HPLC Method using Alumina Filtering to Selectively Extract Phenolic Compounds from Environmental Water

  • Lee, Sung-Kwang
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3755-3759
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    • 2010
  • A on-line SPE (solid phase extraction)-HPLC preconcentration method was developed for the determination of phenolic compounds at trace levels in environmental water sample. XAD-4 and Dowex 1-X8 were used as sorbent in the on-line SPE-HPLC method for the selective enrichment of nine phenolic compounds, which are included in the priority pollutants list of the US EPA. Also alumina prefiltering considerably reduced the amount of interfering peaks due to humic substances that could accumulated due to the preconcentration step and prevent quantification of polar phenolic compounds in environmental water samples. This method was used to determine the phenolic compounds in tap and river water and superiority to the US EPA 625 method in its enrichment factor, pretreatment time, recoveries, and detection limit. The limits of detection were in the range of $0.3-0.9\;{\mu}g/L$ in tap water sample.

Numerical Analysis on Melting and Solidification of Pure Metals with Enthalpy-Porosity Model

  • Kim, Sin;Chung, Bun-Jin;Kim, Min-Chan
    • Journal of Energy Engineering
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    • v.11 no.2
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    • pp.99-105
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    • 2002
  • A finite volume numerical approach is developed and used to simulate convection-dominated melting and solidification problems. The present approach is based on the enthalpy-porosity method that is traditionally used to track the motion of the liquid-solid front and to obtain the temperature and velocity profiles in the liquid-phase. The enthalpy-porosity model treats the solid-phase as the porosity in all computational cells that are located on the solid-liquid interfacial boundary. Concerning the computational cells that are fully located in the solid side of the interfacial boundary, the zero value of the porosity severely suppresses the velocity vector to practically a non-existent value that could be set equal to zero. A comparative analysis with the previous numerical approaches is performed to demonstrate the improved features of the presented model. Results of a melting and solidification experiments are also used to assess and evaluate the performance of the model.

Numerical Analysis of Solid Propellant Ignition ~Numerical Formulation Assessment~

  • Shimada, Toru;Novozhilov, Boris V.
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2004.03a
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    • pp.528-531
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    • 2004
  • For a simple one-dimensional ignition problem a mathematical model is described to investigate the difficulties in numerical simulations. Some computation results are obtained and comparison is made with analytical solution. Discussions are made on topics such as 1) coordinate transformation, 2) gas-phase and solid-phase analysis; (divergence form of the governing system, a finite-volume discretization, implicit time integration, upwind split flux, spatial accuracy improvement are described. Mass, reagent mass, and energy conservations are solved.), and 3) method to determine quantities on the burning surface (matching). Results obtained for small values of the non-dimensional pressure show a steady-combustion and good agreement with the analytical solution. Numerical instability appeared for larger values of the pressure, discussion on the cause of the problem is made. This effort is a part of a study of flame spread phenomena on solid propellant surface.

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Solid Electrochemical Method of Measuring Hydrogen Concentration with O2-/H+ Hetero-Ionic Junction

  • Chongook Park
    • Journal of Sensor Science and Technology
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    • v.33 no.2
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    • pp.63-69
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    • 2024
  • A novel method for measuring hydrogen concentration is introduced, along with its working principle and a novel detection algorithm. This configuration requires no additional reference compartment for potentiometric electrochemical measurements; therefore, it is the most suitable for measuring dissolved hydrogen in the liquid phase. The sensor's electromotive force saturates at a certain point, depending on the hydrogen concentration during the heating process of the sensor operation. This dynamic temperature scanning method provides higher sensitivity than the constant temperature measurement method.

A Study on the Crystallization of Low Density Polyethylene Microparticles in $n$-Dodecanol Solution ($n$-Dodecanol 용액에서 저밀도폴리에틸렌 마이크로 입자 결정화에 관한 연구)

  • Park, Keun-Ho;Jang, Young-Min
    • Journal of the Korean Applied Science and Technology
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    • v.28 no.3
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    • pp.306-312
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    • 2011
  • In this study, we are crystallized to the low density polyethylene (LDPE) micro-particles in $n$-dodecanol solution by thermally induced phase separation(TIPS) method. The Low density polyethylene micro-particles is used in a wide variety of polymer coatings and industrial application. The utility of that for a particular application depends on a number of factors such as the particle size and distribution, and chemical composition of the materials. However, there are still needs for new methods of preparation which will provide the structure with unique sizes. The widely used processes for micro-size particles are crystallization method and thermally induced phase separation. TIPS process based on the phase separation mechanism was performed for the LDPE system which undergoes liquid-solid phase separation. Effects of various operating parameters were examined on the structure variation of the particles. Professionality, take-up speed and crystallization rate depended on temperature and concentration of polymer in solution.