• 제목/요약/키워드: packed column

검색결과 317건 처리시간 0.026초

On-line Trace Enrichment for the Determination of Insulin in Biological Samples Using Reversed-Phase High Performance Liquid Chromatography with Column Switching

  • Lee, Jung-Sook;Lee, Heeyong;Lee, Hye-Suk;Lee, Kang-Choon
    • Archives of Pharmacal Research
    • /
    • 제17권5호
    • /
    • pp.360-363
    • /
    • 1994
  • Column--swtiching technique with a reversed-phase high performance liquid chromatographic method has been developed for the routine analysis of radioiodinated insulin and its degadation products in biological fluids. The diluted biological samples were loaded onto a precolumn packed with LiChrosorb RP-8 $(25-40{\;}{\mu}m)$ using 0.1% trifuoroacetic acid (TFA) in water as a washing solvent. After valve switching, the concentrated insulins were eluted in the back-flush mode and separated by a W-Porex $C_{18}$ column with a gradient of 0.1% TFA in water and 0.1% TFA in acetonitrile as the mobile phase. The method showed good precision, accuracy and speed with the detection limit of 20 pg/ml. Total analysis time per sample was about 40 min and the coefficients of variation were less than 8, 2%.

  • PDF

축방향과 반경방향흐름 크로마토그래피의 단백질 분리속도와 분리능에 대한 비교 (Comparison of Axial and Radial Flow Chromatography on Protein Separation Speed and Resolution)

  • 김윤하;이은규
    • KSBB Journal
    • /
    • 제10권5호
    • /
    • pp.482-490
    • /
    • 1995
  • The relationship between pressure drop and liquid flow rate, for an axial and a radial flow chromatographic column packed with compressible porous media was theoretically analyzed using modified Kozeny-Carman equation. The results were compared with experimental observations obtained using compressible DEAE-agarose as a model medium. At 2-9 psi range studied, the theoretical derivation accounting for 'gel compression' effect predicted simple Langmuirian type response of volumetric flow rate to changes in pressure drop. On the other hand, the experimental response was more or less sigmoidal. At the same pressure drop, radial column showed 2-3 times higher flow rates than those of axial column both theoretically and experimentally. Using r-HBsAg crude extract, protein resolution effects between the two types of columns at different flow rates were compared side-by-side. It turned out that, though general chromatographic behavior was very similar, axial column was somewhat superior in terms of r-HBsAg recovery yield and specificity. However, the number of theoretical plates analysis indicated the protein resolution effects were comparable.

  • PDF

Methylisothiocyanate를 이용한 아미노산 배열결정시 N(O)-butyldimethylsilyl 유도체로서의 methylthiohydantoin 아미노산의 기체 크로마토그래피에 의한 분석 (Gas-chromatographic determination of methylthiohydantoin amino acid as N(O)-butyldimethylsilyl derivatives in amino acid sequencing with methylisothiocyanate)

  • 우강융
    • Applied Biological Chemistry
    • /
    • 제35권2호
    • /
    • pp.132-138
    • /
    • 1992
  • Methylisothiocyanate에 의한 단백질의 아미노산 배열 결정시 순차적으로 분리되어 나오는 methylthiohydantion 아미노산을 기체 크로마토그라피로 효과적으로 정성 및 정량하기위하여 새로운 silylating reagent인 N-methyl-N-(tert.-butyldimethylsily)trifluoroacetamide를 사용하여 N-tert.-butyldimethylsily MTH 유도체로 silylation 한 후 HP-1 capillary column으로 분석하였다. Cystine을 제외한 21개의 단백질 구성 아미노산을 동정할 수 있었고 지금까지 packed column에서 TMS 유도체로 동정할 수 없었던 arginine도 분리 동정되었다. 2개 이상의 peak를 나타낸 것으로는 hydroxyproline, proline, isoleucine, glycine 및 tyrosine이었고 이중 hydroxyproline은 많은 수의 peak들로 분리되었다. Lysine, histidine 및 arginine은 주입량 $5.0\;nmole{\sim}15.0\;nmole$의 범위에서 나머지는 $2.5\;nmole{\sim}7.5\;nmole$의 범위에서 상관관계를 측정한 결과 고도의 직선 상관관계를 나타내었다(p<0.001). TMS 유도체에 의한 분석은 많은 불순 peak들 때문에 정량분석에 이용할 수 없었다.

  • PDF

Effects of Column Length and Particle Diameter on Phospholipid Analysis by Nanoflow Liquid Chromatography-Electrospray Ionization-Mass Spectrometry

  • Lee, Ju-Yong;Lim, Sang-Soo;Moon, Myeong-Hee
    • Mass Spectrometry Letters
    • /
    • 제2권3호
    • /
    • pp.65-68
    • /
    • 2011
  • The effects of column length and particle size on the efficiency of separation and characterization of phospholipids (PLs) are investigated using nanoflow liquid chromatography-electrospray ionization-tandem mass spectrometry (nLC-ESI-MS-MS). Since PLs are associated with cell proliferation, apoptosis, and signal transduction, it is of increasing interests in lipidomics to establish reliable analytical methods for the qualitative and quantitative profiling of PLs related to biomarker development in adult diseases. Due to the complexity of PLs, the preliminary separation of PLs is necessary prior to MS analysis. In this study, length of capillary column and the particle size of reversed phase ($C_{18}$) packing materials are varied to find a reliable condition for the high speed and high resolution separation using 8 PL standard mixtures. From experiments, it was found that a capillary column of nLC-ESI-MS-MS analysis for PL mixtures can be minimized to a 5 cm long pulled tip column packed with 3 ${\mu}m$ $C_{18}$ particles without losing resolution.

Micro-HPLC에 의한 Carbendazim과 Carbaryl의 분석 (Analysis of Carbendazim and Carbaryl by Micro-HPLC)

  • 최경숙;이호연;이덕희;변운기
    • 분석과학
    • /
    • 제7권3호
    • /
    • pp.421-425
    • /
    • 1994
  • A micro-high performance liquid chromatography(Micro-HPLC) techniquie with solid phase extraction was reported which detected carbendazim and carbaryl at picogram levels. They were separated on microbore packed $C_{18}$ column($1.0mm\;I.\;D{\times}150mm$, $d_f=5{\mu}m$) using a 50% methanol mobile phase and detected at UV 220nm(${\alpha}=2.94$, $R_s=4.71$), while they were not resolved on analtical HPLC system(${\alpha}=1.27$, $R_s=0.76$). The detection thresholds of carbendazim and carbaryl were 0.5ng and 0.1ng on Micro-HPLC, therefore Micro-HPLC system was 20~40 told more sensitive than anayltical HPLC system. Sep-Pak $C_{18}$ catridge was found to be efficient in enriching carbendazim and carbaryl from dilute aqueous solution with 97.0% and 97.8% recoveries of them. The Sep-Pak $C_{18}$ catridge followed by the Micro-HPLC had been applied to the quantitative analysis of carbendazim and carbaryl in spiked juices and a commercial drinking water.

  • PDF

흐름식 아임계수에 의한 경유오염토양의 정화 (Remediation of Diesel Contaminated Soil Using Flowing Subcritical Water)

  • 이광춘;정선국;정선용;조영태;박정훈
    • 한국지하수토양환경학회지:지하수토양환경
    • /
    • 제16권3호
    • /
    • pp.10-16
    • /
    • 2011
  • The experimental studies for remediation of diesel contaminated soils were performed using subcritical water in laboratory scale. Contaminated soils from industrial area and artificially contaminated soils were utilized for soil remediation. Experimental system was composed for subcritical water to flow upward through the soil packed column for extracting contaminants. 10 g of contaminated soil was packed into the column and water flow rate was 2 mL/min. To evaluate the effects of temperature, pressure and treatment time on the removal efficiency, temperature was changed from 100$^{\circ}C$ to 350$^{\circ}C$, pressure from 50 bar to 220 bar and treatment time at the predetermined temperature from 0 min to 120 min. The purification efficiency increased as temperature increased. However, the effect of pressure and treatment time was low. Temperature 250$^{\circ}C$, pressure 50 bar and treatment time 30 min were selected for optimal operating condition for this study.

NUMERICAL ANALYSIS OF A SO3 PACKED COLUMN DECOMPOSITION REACTOR WITH ALLOY RA 330 STRUCTURAL MATERIAL FOR NUCLEAR HYDROGEN PRODUCTION USING THE SULFUR- IODINE PROCESS

  • Choi, Jae-Hyuk;Tak, Nam-Il;Shin, Young-Joon;Kim, Chan-Soo;Lee, Ki-Young
    • Nuclear Engineering and Technology
    • /
    • 제41권10호
    • /
    • pp.1275-1284
    • /
    • 2009
  • A directly heated $SO_3$ decomposer for the sulfur-iodine and hybrid-sulfur processes has been introduced and analyzed using the computational fluid dynamics (CFD) code CFX 11. The use of a directly heated decomposition reactor in conjunction with a very high temperature reactor (VHTR) allows for higher decomposition reactor operating temperatures. However, the high temperatures and strongly corrosive operating conditions associated with $SO_3$ decomposition present challenges for the structural materials of decomposition reactors. In order to resolve these problems, we have designed a directly heated $SO_3$ decomposer using RA330 alloy as a structural material and have performed a CFD analysis of the design based on the finite rate chemistry model. The CFD results show the maximum temperature of the structural material could be maintained sufficiently below 1073 K, which is considered the target temperature for RA 330. The CFD simulations also indicated good performance in terms of $SO_3$ decomposition for the design parameters of the present study.

Micro Pre-concentration and Separation of Metal Ions Using Microchip Column Packed with Magnetic Particles Immobilized by Aminobenzyl Ethylenediaminetetraacetic Acid

  • Kim, Y.H.;Kim, G.Y.;Lim, H.B.
    • Bulletin of the Korean Chemical Society
    • /
    • 제31권4호
    • /
    • pp.905-909
    • /
    • 2010
  • Magnetic beads (Dynabeads$^{(R)}$) embedded in ~1 micron size polystyrene beads bearing surface carboxylic acid groups were modified with aminobenzyl ethylenediaminetetraacetic acid (ABEDTA) to concentrate or separate metal ions using pH gradients on micro and nano scales. The immobilization of ABEDTA was achieved by amide formation. The presence of the metal chelating functional group in the fully deprotonated form was confirmed by FT-IR. The chelation efficiency of beads was tested by determining metal ions in supernatant using GFAAS when pH gradients from 3 to 7. Mixtures of Cu and Mg and of Cd and Mn (at 10 ng/mL of metal) were separated as the difference in formation constant with the functional group of ABEDTA. The separation was repeated twice with relative standard deviation of <18%. A polydimethylsiloxane (PDMS) microchip column packed with EDTA-coated magnetic beads was optimized to concentrate metal ion for practical applications by eluting a Cu solution of micro scale at pH 3.

표면개질된 소나무 수피를 이용한 수용액의 구리이온 흡착 (Adsorption of copper ions from aqueous solution using surface modified pine bark media)

  • 박세근;김영관
    • 상하수도학회지
    • /
    • 제33권2호
    • /
    • pp.131-140
    • /
    • 2019
  • This study used a packed column reactor and a horizontal flow mesh reactor to examine the removal of copper ions from aqueous solutions using pine bark, a natural adsorbent prepared from Korean red pine (Pinus densiflora). Both equilibrium and nonequilibrium adsorption experiments were conducted on copper ion concentrations of 10mg/L, and the removals of copper ions at equilibrium were close to 95%. Adsorption of copper ions could be well described by both the Langmuir and Freundlich adsorption isotherms. The bark was treated with nitric acid to enhance efficiency of copper removal, and sorption capacity was improved by about 48% at equilibrium; mechanisms such as ion exchange and chelation may have been involved in the sorption process. A pseudo second-order kinetic model described the kinetic behavior of the copper ion adsorption onto the bark. Regeneration with nitric acid resulted in extended use of spent bark in the packed column. The horizontal flow mesh reactor allowed approximately 80% removal efficiency, demonstrating its operational flexibility and the potential for its practical use as a bark filter reactor.

Study on the Performances of Air Flow Fate Effect on a Structured Packed Tower at Adiabatic Condition in a Liquid Lithium Chloride Cooling System

  • Bakhtiar, Agung;Choi, K.H.;Kim, J.R.
    • 한국태양에너지학회:학술대회논문집
    • /
    • 한국태양에너지학회 2009년도 추계학술발표대회 논문집
    • /
    • pp.404-408
    • /
    • 2009
  • The liquid desiccant air-conditioning system has been proposed as an alternative to the conventional vapor compression cooling systems to control air humidity. The complete system of liquid desiccant air-conditioning system is consisted two main components those are humidifier (regeneration) and dehumidifier. Humidifier part is connected to the load when summer season which is the air condition is hot and humid have to be turned into comfort condition on human. This paper purpose is performances study of air flow rate effect on a structured packed tower on cooling and dehumidifier system using liquid lithium chloride as the desiccant. Experimental apparatus used in this present study is consisted of three components those are load chamber, packed tower and chiller. Load chamber’s volume is $40m^3$, and packed tower dimension is cubic with length 0.4m occupied with packed column. Totally, 15 experimental has done using 5 times repeat on each variable of air velocity that varying on 2m/s, 3m/s and 4m/s with other conditions are controlled. Air inlet initial temperature and relative humidity are set respectively on $30^{\circ}C$ and 52%, desiccant flow rate is 0.63 kg/s, desiccant temperature is $10^{\circ}C$ and desiccant concentration is 0.4. The result of this study shows that averagely, the moisture removal rate and the heat transfer rate are influenced by the air velocity. Higher air velocity will increase the heat transfer and decreasing the moisture removal rate. At adiabatic condition the air velocity of 2 m/s respectively is having the higher moisture removal rate acceleration then the air velocity of 3m/s and 4 m/s until the steady state condition.

  • PDF