• 제목/요약/키워드: size exclusion chromatography

검색결과 131건 처리시간 0.044초

Size-exclusion Chromatography를 활용한 가공식품 중 폴리아크릴산나트륨 분석법 확립 (Analytical Method for Sodium Polyacrylate in Processed Food Products by Using Size-exclusion Chromatography)

  • 정은정;최유정;이근영;윤상순;임호수;김미경;김용석
    • 한국식품위생안전성학회지
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    • 제33권6호
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    • pp.466-473
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    • 2018
  • 가공식품에서 폴리아크릴산나트륨에 대한 분석 방법을 size-exclusion chromatography를 사용하여 개발하고 유통 중인 가공식품에 대해 모니터링 하였다. 분석조건에 대하여 GF-7M HQ column과 UV / VIS 검출기를 피크 모양과 선형성을 기준으로 선택하였으며, 유속, column oven 온도 및 이동상은 각각 0.6 mL/min, $45^{\circ}C$ 및 50 mM sodium phosphate buffer (pH 9.0)으로 선정되었다. 시료의 전처리를 위하여 pH 7.0의 50 mM sodium phosphate buffer로 $20^{\circ}C$, 150 rpm에서 3 시간 동안 추출하였다. 확립된 분석법을 검증한 결과 적절한 선택성을 나타내었으며, 검량선은 50~500 mg/L의 범위에서 선정되었고, 이때 검량선의 상관계수($R^2$)는 0.9985로 나타났다. 폴리아크릴산나트륨의 검출한계(LOD)는 10.95 mg/kg으로 정량한계(LOQ)는 33.19 mg/kg의 값을 얻었으며, 정밀도는 intra-day의 경우 3.0~8.3%를, inter day의 경우 1.3~2.6%로 확인되었다. 정확도는 intra-day의 경우 99.6~127.6%를 나타내었으며, interday의 경우 94.3~121.9%로 확인되었다. 유통 중인 가공식품 125품목을 대상으로 폴리아크릴산나트륨의 함유량을 분석한 결과 40품목에서 검출되었으며, 검출량은 식품첨가물공전의 규격인 0.2% 미만으로 검출되었다. 본 연구결과는 size-exclusion chromatography에 의한 분석방법이 가공식품에서 폴리아크릴산나트륨을 분석하는데 적용할 수 있는 적합한 방법이라는 것을 나타내었다.

기존수처리 공정 및 고도정수처리 공정에서 NOM의 분자크기 분포 변화 (Molecular Size Distributions of NOM in Conventional and Advanced Water Treatment Processes)

  • 최일환;정유진
    • 한국물환경학회지
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    • 제24권6호
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    • pp.682-689
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    • 2008
  • The purpose of this study was to find out the variation between molecular size distribution (MSD) of natural organic matter (NOM) in raw waters after different water treatment processes like conventional process (coagulation, flocculation, filtration) followed by advanced oxidation process (ozonation, GAC adsorption). The MSD of NOM of Suji pilot plant were determined by Liquid Chromatography-Organic Carbon Detection (LC-OCD) which is a kine of high-performance size-exclusion chromatography (HPSEC) with nondispersive infrared (NDIR) detector and $UV_{254}$ detector. Five distinct fractions were generally separated from water samples with the Toyopearl HW-50S column, using 28 mmol phosphate buffer at pH 6.58 as an eluent. Large and intermediate humic fractions were the most dominant fractions in surface water. High molecular weight (HMW) matter was clearly easier to remove in coagulation and clarification than low molecular weight (LMW) matter. Water treatment processes removed the two largest fractions almost completely shifting the MSD towards smaller molecular size in DW. No more distinct variation of MSD was observed by ozone process after sand filtration but the SUVA value were obviously reduced during increase of the ozone doses. UVD results and HS-Diagram demonstrate that ozone induce not the variation of molecular size of humic substance but change the bond structure from aromatic rings or double bonds to single bond. Granular activated carbon (GAC) filtration removed 8~9% of organic compounds and showed better adsorption property for small MSD than large one.

High Temperature Size Exclusion Chromatography for High Throughput Analysis

  • Chang, Tai-Hyun;Park, Soo-Jin;Cho, Hee-Sook;Kim, Young-Tak;Ihm, Kyu-Hyun
    • 한국고분자학회:학술대회논문집
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    • 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
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    • pp.202-202
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    • 2006
  • With a modern size exclusion chromatography (SEC) column, molecular weight analysis of a polymer sample takes about 10 min. However, it is desirable to reduce the analysis time further, in particular, for high throughput measurements required in combinatorial analyses or 2D-HPLC analyses. We implemented the high temperature SEC for the purpose. By inserting a narrow bore tubing between the column and the detector, a sufficient backpressure can be maintained to prevent the mobile phase from boiling and the effluent is cooled down enough when it reaches the detector. Therefore, a normal SEC detector can be used without any modification. The SEC resolution is greatly improved at the elevated temperature at high flow rate which allows high speed operation.

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Trends in Polymer Separations: Better and More Information on Polymer Distributions

  • Schoenmakers, Peter
    • 한국고분자학회:학술대회논문집
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    • 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
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    • pp.113-113
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    • 2006
  • Polymer separations are used to obtain information on molecular distributions (molecular-weight distribution, chemical-composition distribution, functionality-type distribution, etc.). The existing methods, such as size-exclusion chromatography are reliable, but imperfect. New methods and improvements to existing methods are being studied and some of the results will be discussed. In addition, comprehensive two-dimensional liquid chromatography allows the complete characterization of two mutually dependent distributions. LCxSEC chromatograms provide a very good qualitative impression of the distributions, but calibration is not straightforward. Finally, progress in mass spectrometry allows much better information to be obtained.

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Production of selenium peptide from yeast

  • 김영옥;김은기
    • 한국생물공학회:학술대회논문집
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    • 한국생물공학회 2002년도 생물공학의 동향 (X)
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    • pp.208-210
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    • 2002
  • Baker's yeast was cultured with $Na_2SeO_3$. Selenium compounds in yeast were extracted and analyzed by size exclusion chromatography. Selenium was broadly distributed in the fraction of protein. For the inhibition test of MMP-l induction, selenium containing compounds was fractioned by ultrafiltration

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SEC/Light Scattering Analysis of Multicomponent Polymer Systems

  • 이희정;장태현
    • Bulletin of the Korean Chemical Society
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    • 제17권7호
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    • pp.648-653
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    • 1996
  • We have shown several examples of characterization of multicomponent polymer systems by size exclusion chromatography coupled with a light scattering detector. Although SEC cannot provide a complete information for such systems due to its intrinsic limitation, one can extend its capability by combining multiple detection in order to get relevant information to some extent.

Structural and Physiological Characteristics of Rhamnogalacturonan II from Fruit Wines

  • Park, So-Yeon;Shin, Kwang-Soon
    • Food Science and Biotechnology
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    • 제16권2호
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    • pp.270-274
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    • 2007
  • To characterize the polysaccharides which exist as soluble forms in fruit wines, crude polysaccharides were isolated from red, white, raspberry, wild grape, and pear wine, respectively. Among them, the crude polysaccharide (RW-0) in red wine showed the highest yield and considerable amounts of thiobarbituric acid (TBA)-positive materials. The pectic polysaccharide RW-2 was purified to homogeneity from RW-0 by subsequent size-exclusion chromatography using Sephadex G-75 and its structure was characterized. RW-2 consisted of 14 different monosaccharides which included rarely observed sugars in general polysaccharides, such as 2-O-methyl-fucose, 2-O-methyl-xylose, apiose (Api), 3-C-carboxy-5-deoxy-L-xylose (aceric acid, AceA), 3-deoxy-D-manno-2-octulosonic acid (Kdo), and 3-deoxy-D-lyxo-2-heptulosaric acid (Dha). Methylation analysis indicated that RW-2 comprised at least 20 different glycosyl linkages such as 3,4-linked fucose, 2,3,4-linked rhamnose, 3'-linked apiose, and 2,3,3'-linked apiose, being characteristic in rhamnogalacturonan II (RG-II). High performance size-exclusion chromatography indicated that RW-2 mainly comprised RG-II of higher molecular weight (12,000), and that the changes of molecular weight to apparent 7,000 under less than pH 2.0 were observed. These analyses indicated that the higher molecular weight polysaccharide in RW-2 was mainly present as a RG-II dimer.

수용성 streptavidin의 Escherichia coli 에서 기능적 발현 (Functional Expression of Soluble Streptavidin in Escherichia coli)

  • 한승희;김형민;임명운;김진규
    • 생명과학회지
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    • 제25권6호
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    • pp.631-637
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    • 2015
  • Streptmyces avidinii에서 발현되는 Streptavidin은 vitamin H인 d-biotin 4분자에 결합하며 해리상수(Kd)가 10−15 M를 나타내는 아주 강한 비공유결합이다. 이러한 streptavidin과 biotin 상호간의 강한 결합력은 수많은 생물체 분자들의 탐지 및 특징을 연구하는데 응용되어져 왔으므로 Escherichia coli에서 수용성 streptavidin의 기능적 발현에 대한 연구는 매우 유용하다. 즉 Escherichia coli에서 streptavidin을 발현시키기 위해 streptavidin유전자를 T7 RNA polymerase/T7 promoter를 이용하는 pET-22b 플라스미드로 클로닝하였다. 또한 N-말단에 pelB leader를 포함하여 발현된 streptavidin의 periplasmic space로 운반하여 수용성 단백질형태의 분비를 촉진하였으며 C-말단에는 6개의 polyhistidine tags를 두어 정제하는데 사용되었다. 정제된 streptavidin단백질은 10-20 mg/ml 의 높은 회수율을 나타내었으며 SDS-PAGE에서 가열하는 경우 변성되어 17 kD인 monomer형태를, 가열하지 않는 경우에는 68 kDa으로 원래의 tetramer형태를 나타내었다. 따라서 streptavidin의 tetramer 구조는 비공유결합에 의해 이루어짐을 알 수 있었다. Size-exclusion chromatography에 의한 streptavidin의 구조 역시 tetramer를 재확인할 수 있었다. 정제된 수용성 streptavidin은 Westernblot실험에서 biotinylation된 단백질을 탐지하였으며 이 결과는 정제된 streptavidin이 biotin에 결합하는 기능이 존재함을 나타내었다. 이상의 모든 결과를 종합해보면 본 연구에서 구축된 발현시스템을 통하여 발현된 streptavidin은 높은 회수율을 나타내어 대량생산이 가능하였으며 자연상태의 streptavidin과 동일한 homotetramer를 형성하고 biotin에 결합할 수 있는 기능을 나타내었다.

매생이 유래 올리고당의 추출 분리 및 Angiotensin I Converting Enzyme 저해능 분석 (Analysis of Angiotensin I Converting Enzyme Inhibitory Activity of Oligosacchride Extracted from Capsosiphon fulvescens)

  • 김현우;이중헌
    • KSBB Journal
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    • 제28권2호
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    • pp.131-136
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    • 2013
  • The hydrolysates prepared with various enzyme digestion of Capsosiphon fulvescens were used to measure the inhibitory effects against angiotensin I converting enzyme (ACE). The commercially available enzymes such as Celluclast, Viscozyme, Lysing enzyme, Flavourzyme, Alcalase and Pectinex were used to digest C. fulvescens and produce hydrolysates. The maximum ACE inhibitory activity was observed using Alcalase hydrolysis (72.9%). The optimal conditions of Alcalase extraction were pH 8.0 and extraction time for 12 hr. The hydrolysates were fractionated using preparative-LC and anion-exchange chromatography on DEAE-cellulose and the fraction B and B-2 were isolated. The ACE inhibitory activity of fraction B-2 by anion-exchange chromatography was 82.6%. The molecular weight of fraction B-2 estimated using size exclusion chromatography was about 1 kDa. The monosaccharide composition of the fraction B-2 was determined to be mannose (1.1%), glucuronic acid (1.3%), galactose (1.3%) and glucose (96.3%).

Methyl Linoleate 산화중 중합체 형성에 미치는 온도의 영향 (Effect of Temperature on Formation of Polymer in Oxidation of Methyl Linoleate)

  • 김인환;김철진;김동훈
    • 한국식품과학회지
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    • 제28권3호
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    • pp.446-450
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    • 1996
  • Methyl linoleate의 중합체 형성에 미치는 온도의 영향을 조사하기 위해 산소를 주입하인서 $60^{\circ}C,\;90^{\circ}C,\;120^{\circ}C,\;150^{\circ}C$)에서 산화시켰다. 각 온도에서 시간에 따른 과산화물가의 변화 곡선을 기초로하여 각 온도에서 4가지의 산화 시간을 선정하였다. 중합체 함량 및 중합체 결합 특성은 High Performance Size Exclusion Chromatography로 분석하였다. 각 온도에서 만화 시간에 따른 총 산화물 함량과 중함체 함량사이에는 높은 상관관계를 나타냈다. 모든 온도에서 생성된 중합체는 이중체로 확인되었으며, $60^{\circ}C$$90^{\circ}C$에서는 C-O-O-C 결합상태인 이중체를 확인할 수 있었으나, $120^{\circ}C$$150^{\circ}C$에서는 C-O-O-C결합형태를 갖는 이중체는 확인할 수 없었다. 따라서 $120^{\circ}C$$150^{\circ}C$에서 생성된 이중체는 C-O-C/C-C결합 형태인 것으로 추정되었다. 또한, C-O-O-C결합 형태의 이중체는 $60^{\circ}C$보다는 $9^{\circ}C$에서 보다 쉽게 파괴되는 경향을 나타냈다.

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