• Title/Summary/Keyword: 추출크로마토그래피법

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Development of Radiochemical Analysis of Uranium Isotopes in Soil Samples with Extraction Chromatography (크로마토 그래피 추출법을 사용한 토양시료중 우라늄 동위원소 화학분석법 개발)

  • Lee, Myung-Ho;Choi, Guk-Sik;Cho, Young-Hyun;Lee, Chang-Woo;Lee, Soo-Yong
    • Journal of Radiation Protection and Research
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    • v.26 no.1
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    • pp.1-6
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    • 2001
  • An accurate and rapid analytical technique of uranium isotopes in highly contaminated soil samples was developed and validated by application to the IAEA-Reference samples. For overcoming the demerits of the TBP extraction method, sample materials were decomposited with $HNO_3$ and HF, and uranium isotopes were purified by an anion exchange resin and a TRU Spec resin. With the extraction chromatography method, the hindrance elements were completely removed from the uranium fraction. The chemical yields with the extraction chromatography method were more 10% higher than those with the TBP extraction method. The concentrations of uranium isotopes in soil samples using the extraction chromatography method were consistent with the reference values reported by the IAEA.

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Determination of oxymatrine in Sophora Radix by High Performance Liquid Chromatography (고성능 액체 크로마토그래피를 이용한 고삼 중의 oxymatrine 분석에 관한 연구)

  • Yang, Seung Kwon;Yun, Young Ja;Namgung, Mi Ok
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.289-294
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    • 2004
  • A high performance liquid chromatographic method was designed for the quantitative analysis of oxymatrine in Sophora Radix. The separation of oxymatrine was performed by reversed-phase chromatography with a $C_{18}$ column and a buffered aqueous solution containing acetonitrile, and monitored by UV absorption at 215 nm. Extraction of oxymatrine in Sophora Radix was carried out using various solvents and extraction methods. The optimum extraction efficiency for the crushed Sophora Radix was achieved by reflux at $80^{\circ}C$ in 50% ethanol for five hours. Most extraction methods used to complicate pretreatments. In this study, sublimation was employed for a extraction method without going through complicate pretreatments. Sublimation was carried out under high vacuum ($1{\times}10^{-3}$ torr) and at high temperature ($200^{\circ}C$). Extraction efficiency using Sublimation was found to be inferior to other extraction methods.

Determination of Polybrominated Diphenyl Ethers(PBDEs) in Soil using Gas Chromatography/Isotope Dilution Mass Spectrometry (기체크로마토그래피/동위원소 희석 질량분석법을 이용한 토양 중 폴리브롬화 디페닐에테르의 분석법)

  • Na, Yuncheol;Chang, Yoon-Seok;Kim, Hai-Dong;Hong, Jongki
    • Analytical Science and Technology
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    • v.17 no.1
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    • pp.29-36
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    • 2004
  • An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.

Gas-Liquid Chromatographic Determination of Haloxyfop-R and lts Methyl Ester Residues in Soils and Soybeans (토양과 대두중 Haloxyfop-R 및 Haloxyfop-R-methyl의 기체크로마토그래피를 이용한 잔류분석)

  • Lee, Young-Deuk
    • Korean Journal of Environmental Agriculture
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    • v.16 no.4
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    • pp.333-340
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    • 1997
  • An analytical method was developed to determine residues of haloxyfop-R and its methyl ester in soils and soybeans using gas-liquid chromatography (GLC) with electron capture detector (ECD). Soil or soybean sample was acidified and extracted with acetone. The extract was then subjected to ion-associated partition to individually separate haloxyfop-R and the neutral methyl ester. One phase containing haloxyfop-R was methylated with $BF_3$/methanol, partitioned to n-hexane and analyzed by GLC/ECD. The other phase containing the methyl ester was further purified by Florisil column chromatography prior to GLC determination. No cross contamination was found between two phases containing each of the acid and methyl ester, thus two compounds can be separately determined as the identical haloxyfop-R-methyl. Overall recoveries of haloxyfop-R from fortified samples averaged 88.2${\pm}$3.9% (n=12) and 88.3${\pm}$4.0% (n=6) for soils and soybeans respectively, and those of haloxyfop-R-methyl showed mean values of 89.2${\pm}$4.0% (n=12) and 85.6${\pm}$5.6% (n=6). Detection limits of both haloxyfop-R and its methyl esterwere 0.005㎎/㎏ and 0.01㎎/㎏ for soil and soybean samples respectively.

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Single step purification of potent antigenic protein from sparganum by gelatin-affinity chromatography (젤라틴 친화성 크로마토그래피를 이용한 스파르가눔 성분단백질의 순수분리)

  • Yoon Kong;Shin-Yong Kang;Seung-Yull Cho
    • Parasites, Hosts and Diseases
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    • v.29 no.1
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    • pp.1-8
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    • 1991
  • Out of many component proteins in crude saline extract of Spirometra mansoni plerocercoid (sparganum) , 36 kDa and 29 kDa proteins were found to be the most antigenic and were already purified by immunoaffinity chromatography using monoclonal antibody as a ligand. In this study, a single step purification of these potent antigenic proteins of sparganum extract was investigated. When the crude saline extract was charged to gelatin-Sepharose 4B affinity column, 36 kDa and 29 kDa protein fractions were bound. SDS-polyacrylamide gel electrophoresis (PAGE) and SDS-PAGE/immunoblot confirmed that the bound protein to gelatin was serologically pure. When evaluated by ELISA with patients sera, the purified protein of 36 and 29 kDa also showed improved antigenicity.

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Antioxidant activity of ethanol extract and methanol fractions via column chromatography from Psidium guajava Leaf (구아바 잎 추출물 및 컬럼크로마토그래피를 이용한 메탄올 분획물의 항산화 활성)

  • Byeoung-Kyu Choi
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.266-271
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    • 2023
  • The antioxidant capacity of the Psidium guajava leaf extracted with EtOH and their MeOH fractions using column chromatography were evaluated by 1,1-diphenyl-2-picrylhydrazyl and 2,2'-azino-bis-3-ethylbenzothiazoline-6-sulfonic acid radical scavenging assays, total phenolic and flavonoid content, and Superoxide dismutase (SOD) assay. To determine its utility as a functional material, the crude extract was fractionated by flash column chromatography on ODS using a stepwise elution with combinations of MeOH/H2O and then all the fractions were also investigated. In the results of antioxidant activities, the 40% and 60% MeOH fractions show the meaningful values, and then the two fractions were selected to examine the isolation and identification of the major constituents via HPLC and nuclear magnetic resonance. Further purification led to isolation of two quercetin derivatives; quercitrin (1) and isoquercetin (2). Through SOD assay, some methanol fractions via column chromatography and isolated compounds showed improved antioxidant activities compared to the extract.

Studies on the Simultaneous Analysis of Organochlorine Pesticide Residues by Gas-Liquid Chromatography (I). Solvent Extraction and Cleanup of Pesticides (기체-액체 크로마토그래피에 의한 잔류 유기염소제 농약들의 동시 분석에 관한 연구 (제1보). 농약의 용매추출 및 불순물 제거)

  • Taek-Jae Kim;Song-Ja Park;Young-Sang Kim
    • Journal of the Korean Chemical Society
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    • v.29 no.5
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    • pp.496-502
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    • 1985
  • The solvent extraction and cleanup processes for the simultaneous gas-liquid cliromatographic determination of 16 kinds of organochlorine pesticide residues were investigated. The pesticides were extracted out from-various crops with the aqueous acetone solution acidified (pH < 1.5) by adding conc. $H_3PO_4$. Most of the pesticides were partitioned from the solution with petroleum ether. Evaporated the extracting solvent, the residues were dissolved in ethylether-petroleum ether (6 : 94) eluent and eluted through the Florisil column activated at 650$^{\circ}$C for 2.5hrs. The extraction efficiency was over 94% and impurities were effectively removed by the column chromatography.

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Molecular Cloning of H-Y Antigen Gene I. Purification of H-Y Antigen by Immunoaffinity Chromatography and Chemiluminescence Immunoassay for the Assay of H-Y Antigen (H-Y 항원 유전자의 cloning에 관한 연구 I. 친화성 크로마토그래피에 의한 H-Y 항원의 분리 정제 및 H-Y 항원 정량을 위한 화학발광 면역 분석법)

  • 김종배;김재홍;백정미;김창규;정길생
    • Korean Journal of Animal Reproduction
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    • v.15 no.2
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    • pp.149-155
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    • 1991
  • 본 실험은 H-Y 항원 유전자 크로닝을 위한 기초연구로서 H-Y 항원의 특성을 규명하기 위하여 친화성 크로마토그래피에 의하여 H-Y 항원을 분리·정제하였다. 정소 추출액을 항체가 결합된 column에 결합시킨 뒤 10% acetic acid로 용출시켰다. 용출된 분획을 모아 농축한 후 HPLC와 SDS-PAGE를 실시하여 H-Y 항원의 분자량은 약 6,7000달톤 임을 알 수 있었으며 isoelectric focusing에 의하여 등전점(pI)은 5.0인 것으로 측정되었다. H-Y 항원에 대한 단일클론항체와 표지항원으로는 H-Y 항원-ABEI(aminobutylethyl isoluminol)를 사용하여 H-Y 항원 정량을 위한 화학발광면역분석법을 개발하였다. 항원항체 반응후 빛의 측정은 NaOH 존재하에서 microperoxidase/H2O2를 이용한 산화반응으로 실시하여 10초간 측정한 빛의 양을 적분하였다. H-Y 항원의 농도와 빛의 양과는 역비례하였으며 감도는 11.8ng/tube 정도이었다.

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The Analysis on VOCs That Occurs in Leather Cultural Heritage with SPME (고체상미세추출법(SPME)을 이용한 피혁 재질로부터 발생된 휘발성 유기화합물 분석기술 연구)

  • Chung, Yong-Jae
    • Journal of Conservation Science
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    • v.28 no.2
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    • pp.113-118
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    • 2012
  • Cultural heritages emit volatile organic compounds(VOCs) during degradation as chemical, biological factors. These VOCs in the atmosphere are degradation factors for another materials. But non-destructive organic analysis methods are uncommon, and have difficulties for field application. In this study, solid phase micro-extraction(SPME) and gas chromatography( GC) are carried out for analysis of VOCs which are emitted from leather, and prove SPME field holder's efficiency. I analize leather archival objects at The National Archives of Korea by cross-checking GC and SPME methods. It could be confirmed that the compounds are (E)-2-nonenal, butyl hydroxy toluene emitted itself from leather.