• 제목/요약/키워드: solid phase method

검색결과 1,186건 처리시간 0.023초

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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    • 제17권3호
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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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    • 제13권2호
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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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    • 제17권4호
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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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가열 조리된 돼지고기의 Heterocyclic Amines 분석을 위한 Solid-phase 추출 방법의 비교 (Comparison of Different Solid-Phase Extraction Methods for the Analysis of Heterocyclic Amines from Pan-Fried Pork Meat)

  • 이재환;백유미;이광근;신한승
    • 한국축산식품학회지
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    • 제28권5호
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    • pp.637-644
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    • 2008
  • 식품 중 HCAs을 검출하기 위한 최적 전처리 방법을 확립하기 위해 가열 조리된 돼지고기 패티를 이용하여 서로 다른 4가지 SPE(solid-phase extraction)방법을 비교하였다. 4가지 전처리 방법을 통해 얻은 15가지 HCAs 회수율은 3.0%(방법 A, Tri-P-1)-74.7%(방법A, Tri-P-2)이었다. 그 중 $MeA{\alpha}C$가 평균적으로 73.4%로 가장 높은 회수율을 보였으며 Tri-MeIQx가 15.2%의 가장 낮은 회수율을 보였다. 4가지 전처리 방법 중 방법A와 방법D가 가장 높은 회수율과 검출빈도를 보였으며 방법B와 방법C는 Harman(14.8%)을 제외하고는 전혀 검출되지 않았고 회수율을 구할 수 없었다 발암 가능 물질인 IQ, $A{\alpha}C$, $MeA{\alpha}C$, Glu-P-1, Glu-P-2, MeIQ, MeIQx, PhIP 등을 검출하는 방법에는 방법A(48.7-74.6%)가 4가지 방법 중 가장 유리하다. HCAs는 극성에 따라 polar amines과 less-polar amines으로 구분할 수 있는데 방법A는 less-polar amines검출에 유리하고 방법D는 polar amines검출에 유리하다. 방법A와 방법D의 chromatogram을 비교한 결과 방법A와 방법D 모두 15가지 HCAs가 깨끗하게 분리되었지만 Tri-MeIQx 등을 검출하는데 방법A가 더욱 유리하다. SPE 전처리 방법 및 LC/MS 분석방법에 대한 유효성을 확인하기 위해 LOD(0.2-2.1 ng/mL)와 LOQ(0.8-9.7 ng/mL), 표준 편차(0.2-8.6)를 구하였다.

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

  • 황기영;이진호
    • 대한기계학회논문집
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    • 제19권4호
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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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    • 제31권12호
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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
    • 에너지공학
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    • 제11권2호
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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.
    • 한국추진공학회:학술대회논문집
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    • 한국추진공학회 2004년도 제22회 춘계학술대회논문집
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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
    • 센서학회지
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    • 제33권2호
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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.

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

  • 박근호;장영민
    • 한국응용과학기술학회지
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    • 제28권3호
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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.