• 대한화학회지
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• 제39권8호
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• pp.635-642
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• 1995

Purge & Trap-GC/MS 전처리 방법과 capillary column gas chromatography/ mass spectrometry 분석법을 이용한 휘발성유기물 분석에 있어서, 보다 효울적으로 시료를 주입하는 방법에 대하여 연구하였다. 미국환경청에서 제시한 물 중의 휘발성 유기물 분석방법에서 이용하는 moisture control nodule 과 cryorefocusing에 따르는 여러가지 문제점을 관찰하였다. 이러한 무제점을 해결하기 위해 개선된 시료 주입방식을 제시하고, 여러가지 트랩과 컬럼의 특성을 조사하여 최적 실험조건을 구하였다. 이때 사용한 Purge & Trap 장치의 트랩은 carbopack B/carboxen 1000과 1001이었으며, 기체 크로마토그라프의 컬럼은 주문 제작한 dimethyldiphenylpolysiloxane crosslingking moiety capillary 컬럼을 사용하였다. 본 연구에서 제시한 방법으로 물 중에 포함된 54종의 휘발성유기물을 대상으로 동시분석할 때의 정확도와 정밀도에 대해 조사하였으며, 각 화합물에 대한 method detection limit를 구하였다.

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.45-50
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• 2014

A fully packed capillary electrochromatographic (CEC) microchip with an on-column micro-solid phase extraction (SPE) bed for the preconcentration and separation of organic analytes was prepared. A linear microchannel with monodisperse colloidal silica packing was formed on a cyclic olefinic copolymer microchip with two reservoirs on both ends. Silver-cemented silica packing frit structure was formed at the entrance of the microchannel by electroless plating treatment as a base layer. A gold coating was formed on it by reducing $Au^{3+}$ to gold with hydroxylamine. Finally micro-SPE bed was formed by self-assembly adsorption of 1-dodecanethiol on it. Micro-SPE beds were about 100-150 ${\mu}m$ long. Approximately $10^3$ fold sensitivity enhancements for Sulforhodamine B, and Fluorescein in nM concentration levels were possible with 80 s preconcentration. Basic extraction characteristics were studied.

• Bulletin of the Korean Chemical Society
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• 제31권10호
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• pp.2934-2938
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• 2010

Some open tubular (OT) molecule imprinted polymer (MIP) silica capillary columns with templates of camphor derivatives such as 10-camphorsulfonic acid (10-CSA), 10-camphorsulfonamide (10-CS) and camphor-p-tosyl hydrazone (CTH) have been successfully prepared by the prior generalized preparation protocol. The three MIP thin layers of different templates showed quite different morphologies. The chiral selectivity of each MIP column for the template enantiomers was optimized by changing eluent composition and pH. The optimization conditions were found to be different for the three MIPs. This work suggests prospective successful extension of the generalized preparation protocol for OT-MIP silica capillary columns toward templates of a variety of chemical groups.

• 분석과학
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• 제11권3호
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• pp.213-221
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• 1998

Bromide, chloride, fluoride, nitrite, nitrate, sulfite, sulfate, perchlorate, chlorate 및 chlorite가 포함된 시료를 capillary zone electrophoresis(CZE)와 indirect UV detection 방법으로 분리하였다. 음이온류의 분리는 running buffer로 5 mM ammonium dichromate, 10 mM ammonium acetate, 20 mM diethylenetriamine, 10% methanol(pH 9.3)을 사용하였으며 전압은 cathode에 15 kV를 공급하였다. 또한 최초로 CZE에서 음이온의 정량이 가능하도록 각 이온들에 대한 regression과 detection limit를 결정하였고, 이 분석방법은 톨루엔을 흡입한 사람의 뇨, 부검 혈액, 폐수 및 폭약 등 시료에 적용하였으며, 음이온의 함량을 ion chromatograph(IC)와 비교 검토하였다.

• 한국전산유체공학회:학술대회논문집
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• 한국전산유체공학회 2005년도 추계 학술대회논문집
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• pp.21-26
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• 2005

Gas Chromatography (GC) is a wisely technique used for the separation and analysis of liquid and gas sample. Separation of the sample vapors is achieved via their differential migration through a capillary column with an insert carrier gas. The identity and quantity of each vapor in the mixer can be determined from its retention time in the column and a particular property of the gas, such as thermal conductivity, which can be related to the concentration of sample vapor in the carrier gas. Therefore, the flow characteristics in the spiral gas chromatographic column are numerically investigated in this study. Especially, different pressure drop between the front and the rear of GC column with various flow rates is estimated the governing equations are derived from making using of three-dimensional Naver-Stokes equation with incompressible and laminar model due to the nature of low Reynolds number flow. Using a commercial code, FLUENT, the pressure and flow fields in GC column are calculated with various flow rates. The characteristics of thermal cycling which is one of the most important factors affecting the column efficiency and analysis time is also estimated. Furthermore, numerical analyses are also carried out by using commercial code, ANSYS, with various values of power, which is applied to the heating element located at lower GC column.

• Applied Biological Chemistry
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• 제32권4호
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• pp.344-349
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• 1989

GC/MS를 이용하여 오미자의 chloroform-methanol 추출물로부터 11종의 lignan 성분을 동정하였다. GC column은 SPB-1 fused silica capillary $(0.25mm\;ID{\times}30m,\;Supelco)$를 사용하였고 column oven의 온도는 $200^{\circ}C$부터 $300^{\circ}C$까지 분당 $4^{\circ}C$씩 승온하였으며 MS의 ionization voltage는 70eV (El mode)이었다. 동정된 lignan 성분은 gomisin J, deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H, tigloylgomisin H, angeloylgomisin Q, gomisin B 및 benzoylgomisin H이었으며, GC chromatogram 상에서 이들 화합물의 분리상태는 양호하였다.

• Applied Biological Chemistry
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• 제35권2호
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• pp.132-138
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• 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.

• Molecular & Cellular Toxicology
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• 제1권2호
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• pp.87-91
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• 2005

Although 2D-PAGE has been widely used as the primary method for protein separation, difficulties in displaying proteins with an extreme values of isoelectric paint (pI), molecular size and hydrophobicity limit the technique. In addition, time consuming steps involving protein transfer and extraction from the gel-pieces can result in sample loss. Here, we describe a novel protein separation technique with capillary size-exclusion chromatography (CSEC) for rapid protein identification from human plasma. The method includes protein fractionation along with molecular size followed by in-solution tryptic digestion and peptide analysis through reversed phase liquid chromatography (RPLC) coupled to nanoflow electrospray-tandem mass spectrometry (ESI-MS/MS). Tryptic peptides are applied an a $100\;{\mu}m\;i.d.{\times}10mm$ length pre-column and then separated on a $75\;{\mu}m{\times}200mm$ analytical column at -100 nL/min flaw rate. Proteins were identified over the wide ranges of pI (3.7-12.3) when this technique was applied to the analysis of $1-2\;{\mu}L$ of human plasma. This gel-free system provides fast fractionation and may be considered a complementary technique to SDS-PAGE in proteomics.

• 공업화학
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• 제25권2호
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• pp.147-151
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• 2014

많은 고분자 공정에서 고분자에서의 유기 용매와 같은 저분자 물질의 확산은 중요하다. 고분자에서의 저분자 물질의 이동은 중합 반응기의 효율성과 제조된 고분자의 특성을 결정한다. 공정을 설계하고 최적화하는데 중요한 물성값은 고분자/용매 상호확산 계수이다. 용매의 농도가 매우 낮은 무한희석 상태에서의 고분자/용매 계의 무한확산계수를 측정하기 위해서 capillary column inverse gas chromatography (CCIGC) 기법이 흔히 사용된다. 이 기법을 사용하면 비교적 짧은 시간에 확산계수와 분배계수를 측정하는 것이 가능하다. 본 연구에서는 CCIGC 기법을 사용해서 styrene/butadiene/styrene (SBS) 블록 공중합체에서 환형 구조를 가지는 용매의 확산계수와 분배계수를 다양한 온도 범위에서 측정하였다.

• Preventive Nutrition and Food Science
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• 제3권2호
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• pp.111-118
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• 1998

To develop a simple, rapid and simultaneous analytical method of phenolic compounds using gas chromatography (GC) and gas chromatography/mass spectrophometer (GC/Ms), this experiment was carried out to search the retention times of capillary columns and the characteristics of fragment ions in electron impact mass spectra. Most of trimethylsilyl derivatives and underivatized phenolic compounds were separated very well on three kinds of capillary columns(HP-1), Ultra-2 and HP-35). Quantitiative determination of phenolic compounds was achieved by internal standards (p-hydroxybenzoic acid iopropyl ester, p-hydroxybenzoic acid ethyl ester). Calibration plts were linear in the investigated range, and the limits of detection were about 5 ng at split mode method. When analyzed by three columns, theseparation times were fairly constant on two nonpolar columns, but a few compounds showed slightly different separation order by the itnermediate polar HP-35 column. The important characteristic patterns of TMS derivatives of phenolic compounds on the EI/MS spectrra appeared at the base peak of [M-15]+ ion and presented at high abundance in most TMS derivatives of phenoloc compounds. [M]+, [M-CH3-COO]+, [M-Si(CH3)4]+ and [M-Si(CH3)4 -CH3]+ also observed in mass spectra of these compounds . Although several compounds have the same retention times on GC column, it might be possible to identify these compounds by the different patternsof mass frgement ions. The TMS derivatives, thus , provide additional information for identification of phenolic compounds in biological systems.