• Bulletin of the Korean Chemical Society
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• 제27권3호
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• pp.413-418
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• 2006

Sodium hyaluronate (NaHA), water soluble polymer having ultra-high molecular weight, is characterized by using on-line frit inlet asymmetrical flow field-flow fractionation (FI-AFlFFF) and multiangle light scattering (MALS). This study demonstrates the capability of power programming FI-AFlFFF for the separation of NaHA and the applicability of FI-AFlFFF with MALS for the characterization of molecular weight distribution and their structural information. Since sample injection and relaxation in FI-AFlFFF are achieved by using hydrodynamic relaxation, separation of high molecular weight polymers can be achieved smoothly without halting the separation flow. Experiments are carried out with the two different NaHA products (a raw NaHA sample and a thermally degraded NaHA product) and molecular weight distribution and conformations in solution are determined. Influence of sample filtration on the change of molecular weight distribution is also discussed.

• Bulletin of the Korean Chemical Society
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• 제32권4호
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• pp.1315-1320
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• 2011

Whey protein (WP) is a mixture of proteins, and is of high nutritional values. WP has become an important source of functional ingredients in various health-promoting foods. In this study, size-exclusion chromatography (SEC) and asymmetrical flow field-flow fractionation (AsFlFFF) were used for separation and analysis of whey proteins. It was found that a lab-prepared WP from raw milk is mostly of ${\beta}$-lactoglobulin with small amount of higher molecular weight components, while a commercial whey protein isolate (WPI) powder contains relatively larger amount of components other than ${\beta}$-lactoglobulin, including IgG and protein aggregates. Results suggest that AsFlFFF provides higher resolution for the major whey proteins than SEC in their normal operation conditions. AsFlFFF could differentiate the BSA and Albumin, despite a small difference in their molecular weights, and also was able to separate much smaller amount of aggregates from monomers. It is noted that SEC was able to show the presence of low molecular weight components other than the major whey proteins in the WP samples, which AsFlFFF could not show, probably due to the partial loss of those low molecular weight species through the membrane.

• 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.

• 분석과학
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• 제32권5호
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• pp.173-184
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• 2019

As the size of semiconductors becomes smaller, it is necessary to perform high precision polishing of nanoscale. Ceria, which is generally used as an abrasive, is widely used because of its uniform quality, but its stability is not high because it has a high molecular weight and causes agglomeration and rapid precipitation. Such agglomeration and precipitation causes scratches in the polishing process. Therefore, it is important to accurately analyze the size distribution of ceria particles. In this study, a study was conducted to select dispersants useful for preventing coagulation and sedimentation of ceria. First, a dispersant was synthesized and a ceria slurry was prepared. The defoamer selection experiment was performed in order to remove the air bubbles which may occur in the production of ceria slurry. Dynamic light scattering (DLS) and asymmetrical flow field-flow fractionation (AsFlFFF) were used to determine the size distribution of ceria particles in the slurry. AsFlFFF is a technique for separating nanoparticles based on sequential elution of samples as in chromatography, and is a useful technique for determining the particle size distribution of nanoparticle samples. AsFlFFF was able to confirm the presence of a little quantities of large particles in the vicinity of 300 nm, which DLS can not detect, besides the main distribution in the range of 60-80 nm. AsFlFFF showed better accuracy and precision than DLS for particle size analysis of a little quantities of large particles such as ceria slurry treated in this study.

• 분석과학
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• 제17권2호
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• pp.163-172
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• 2004

토양 풀빅산 (FA)의 분자량 크기 분포와 분자량별 형광특성을 겔 여과 크로마토그래피(GFC)와 형광분석시스템을 사용하여 분석하였다. 본 연구에서는 제주 지역 토양에서 추출한 풀빅산을 세 개의 분자량 영역으로 분리하였고, 분자량별 풀빅산의 excitation, emission, synchronous 형광특성을 비교 분석하였다. 토양 풀빅산의 분자량 분리를 위한 GFC 시스템은 아세톤과 덱스트란 블루 및 폴리에틸렌 글리콜 표준분자를 사용하여 교정하였다. 분자량 분리 시스템의 틈새부피는 130 mL이고, total permeation volume은 404 mL을 나타냈다. 이 시스템을 풀빅산의 분자량 분리에 적용한 결과, 토양 풀빅산은 190~8,900 Da의 분자량 분포를 나타냈으며 피크점에서의 분자량은 930 Da을 나타냈다. 분자량별 구조 차이를 나타내는 synchronous 형광피크의 상대비 ($I_{498nm}/I_{390nm}$)는 분자량이 클수록 증가하였다. 이와 같은 결과는 고 분자량의 풀빅산이 저 분자량의 풀빅산에 비해 ${\pi}$-결합으로 연결된 방향족 고리와 다양한 치환기가 결합된 좀더 복잡한 분자 구조임을 제시한다.

• 한국환경과학회지
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• 제7권1호
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• pp.104-111
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• 1998

The Dongbok lake water before and after alum coagulation and activated carbon adsorption were analyzed in terms of organic contents, molecular weight distributuin (MWD), and UV-absorbance. Dissolved organic compounds in the Dongbok lake were fractionated into three molecular size classes by gel permeation chromatography. The fractionation was reasonably successful in isolating compounds with The bulk of the dissolved carbon was present in compounds of molecular weight in the range of 3,000~10,000. Alum coagulation preferentially treated molecules of high molecular weight, which has molecules larger than 10,000. The dissolved organic carbon (DOC) removal after activated carbon adsorption was high in the Fraction B , IR . The $A_{260}$/DOC ratio after alum and activated carbon treatment the Fraction II, III. This results suggest that the organics remaining after each treatment has a trihalomethane formation potential

• 한국지하수토양환경학회지:지하수토양환경
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• 제20권7호
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• pp.70-79
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• 2015

A sample of soil humic acid (HA) was divided by ultrafiltration (UF) into five fractions of different molecular size (UF₁: > 300, UF₂: 100~300, UF₃: 30~100, UF₄: 10~30, UF₅: 1~10 kilodaltons). Apparent average molecular weight (M_w) of the HA fractions were measured using high performance size exclusion chromatography (HPSEC), and the chemical and structural properties of the five HA fractions were characterized by elemental compositions (H/C, O/C and w ((2O + 3NH)/ C)) and ultraviolet-visible absorption ratios (SUVA, A_4/6). The organic carbon normalized-sorption coefficients (Koc) for the binding of phenanthrene to the HA fractions were determined by fluorescence quenching and relationship between the sorption coefficients and structural characteristics of the HA fractions were investigated. The elemental analysis and UV-vis spectral data indicated that the HA fractions with higher molecular weights have grater aliphatic character and lower contents of oxygen, while the HA fractions with lower molecular size have greater aromatic character and molecular polarity that correspond to greater SUVA and internal oxidation values (w). The log Koc values (L/kg C) were gradual increased from 4.45 for UF₅ to 4.87 for UF1. The correlation study between the structural descriptors of the HA fractions and log Koc values of phenanthrene show that the magnitude of Koc values positively correlated with $M_w$ and H/C, while negatively correlated with the independent descriptors of the O/C, w, SUVA and A_4/6.

• 한국물환경학회지
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• 제25권2호
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• pp.288-294
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• 2009

Flow field-flow fractionation (Fl-FFF) device has been widely used to verify the size and molecular weight of various colloids and organics. The Fl-FFF, however, generally uses carrier solutions with only low to moderate ionic strengths to exclude the high affinity of materials to the membrane under high ionic strength conditions. Thus, materials existing in seawaters have not been accurately analysed based on the hydrodynamic size and molecular weight using current Fl-FFF techniques. The highest ionic strength tested was up to 0.1 M, while seawater ionic strength is about 0.6 M. The aim of this study is to accurately measure the hydrodynamic size of particles under carrier solutions close to seawater conditions with the Fl-FFF. By employing various operating conditions during the Fl-FFF analyses, it was demonstrated that the flow conditions, the concentration of surfactants, and stabilization times were key factors in acquiring compatible data. Results have shown that the cross flow was more influential factor than the channel flow. The concentration of the surfactant was to be at least 0.05% and the minimum 15 hr of stabilization was needed for accurate and reproducible data acquisition under seawater condition.

• Bulletin of the Korean Chemical Society
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• 제22권4호
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• pp.337-348
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• 2001

This article gives an overview of a recently developed channel system, frit-inlet asymmetrical flow field-flow fractionation (FI-AFlFFF), which can be applied for the separation of nanoparticles, proteins, and water soluble polymers. A conventiona l asymmetrical flow FFF channel has been modified into a frit-inlet asymmetrical type by introducing a small inlet frit near the injection point and the system operation of the FI-AFlFFF channel can be made with a great convenience. Since sample components injected into the FI-AFlFFF channel are hydrodynamically relaxed, sample injection and separation processes proceed without interruption of the migration flow. Therefore in FI-AFlFFF, there is no requirement for a valve operation to switch the direction of the migration flow that is normally achieved during the focusing/relaxation process in a conventional asymmetrical channel. In this report, principles of the hydrodynamic relaxation in FI-AFlFFF channel are described with equations to predict the retention time and to calculate the complicated flow variations in the developed channel. The retention and resolving power of FI-AFlFFF system are demonstrated with standard nanospheres and protreins. An attempt to elucidate the capability of FI-AFlFFF system for the separation and size characterization of nanoparticles is made with a fumed silica particle sample. In FI-AFlFFF, field programming can be easily applied to improve separation speed and resolution for a highly retaining component (very large MW) by using flow circulation method. Programmed FI-AFlFFF separations are demonstrated with polystyrene sulfonate standards and pululans and the dynamic separation range of molecular weight is successfully expanded.

• 대한자원환경지질학회:학술대회논문집
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• 대한자원환경지질학회 2003년도 춘계 학술발표회 논문집
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• pp.69-71
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• 2003

토양 및 수질 유기물질과 금속 산화물사이의 상호 반응관계는 환경지구화학적으로 중요하게 다루어진다 (Sposito, 1984). 토양내 광물들의 표면은 토양 유기물질의 주요한 부분을 차지하는 휴믹물질, 즉 휴믹산과 펄빅산에 의해서 이온강도와 산도에 따라 피복하는 현상을 일으킨다. 특히, 휴믹산과 펄빅산은 토양 및 수질내 주요한 구성 유기물로 존재하며 다양한 유기화합물과 분자량을 갖으며, 중금속들의 유출에 의한 오염 환경에서 그 화학종과 이동도에 영향을 주게된다 (Thurman, 1985). (중략)