• Title/Summary/Keyword: 액체 크로마토그래피

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Separation of Hg(II) by using the poly-NTOE(1, 12-diaza-3, 4:9, 10-dibenzo-5, 8-dioxacyclopentadeca-1, 12-ylene-2, 7-dihydroxyoctamethylene) in Liquid Chromatography (액체 크로마토그래피에서 Poly-NTOE(1, 12-diaza-3, 4:9, 10-dibenzo-5, 8-dioxacyclopentadeca-1, 12-ylene-2, 7-dihydroxyoctamethylene)를 이용한 Hg(II)의 분리)

  • Kim, Hae-Joong;Shin, Young-Kook;Kim, Si-Joong
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.259-264
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    • 1995
  • The separation efficiency of metal ions by using the poly-NTOE(1, 12-diaza-3, 4:9, 10-dibenzo-5, 8-dioxacyclopentadeca-1, 12-ylene-2, 7-dihydroxyoctamethylene) has been determined by column chromatography in aqueous solution. Binding constants and separation factors for several poly-NTOE interactions were measured in aqueous solution. The order of these binding constants and separation factors with metal ions were Co(II)Zn(II) for the transition metal ions and Cd(II)

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Studies on the Development of Liquid Chromatographic Methods for Pesticide Residues (I)-Separation Optimization of Thiocarbamates (잔류농약의 액체 크로마토그래피 분석법 개발에 관한 연구 (I) Thiocarbamates 제초제의 분리 최적화)

  • Lee Dai Woon;Choi Yong Wook;Suh Joon Ha
    • Journal of the Korean Chemical Society
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    • v.36 no.1
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    • pp.57-65
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    • 1992
  • The method for investigating the retention behavior and separation optimization was studied to develop a reversed-phase liquid chromatography of eleven thiocarbamates that are used as herbicides. As an isocratic elution system, the statistical simplex technique was applied to find the optimum separation conditions. The resolution was quantitatively evaluated by using COF and ORM method. For thiocarbamate herbicides in which the elution order varies dramatically with solvent composition, the ORM method gave better result than the COF method. For the solvent composition of mobile phase in the ORM method, the ratio of methanol : acetonitrile : tetrahydrofuran : water was 16 : 29 : 2 : 53. Also in this research, an adjusted COF $(\overline{COF})$ method was proposed to rectify the defect in the current COF method, and the compositional ratio of mobile phase containing methanol : acetonitrile : water was 29.5 : 21.5 : 49.0 result of which is similar to that obtained by the ORM method.

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Determination of Polarity Scales of Mixed Solvents for Normal Phase Liquid Chromatography (정상 액체 크로마토그래피에 사용되는 혼합용매들의 극성도 지수 결정에 관한 연구)

  • Won Jo Cheong;In Ki Kim;Byung Bae Park
    • Journal of the Korean Chemical Society
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    • v.37 no.12
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    • pp.1025-1034
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    • 1993
  • We have measured ${\pi}^*$, $\alpha$ and $\beta$ polarity parameters of 2-propanol / hexane and ethyl acetate / hexane mixed solvents over the entire range of composition. For the ethyl acetate / hexane system, only ${\pi}^*$ and $\beta$ were measured since $\alpha$ of these mixed solvents are defined zero. We have corrected the measured polarity parameters to obtain consistent data with the existing literature data assuming a good linear correlation between the measured and the true values. The variation patterns are consistent with the expected trends based on the chemistry of the solvent components. The general trends of the two solvent systems are summarized as follows. ${\pi}^*$ merely increases as the content of the more polar solvent increases while $\alpha$ and $\beta$ increase with the increase of the content of the more polar solvent, then decrease upon continuing addition of the more polar solvent.

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Studies on the Elution Behavior and the Simultaneous Analysis of Some Metal-Dithiocarbamate Chelates by Reversed-Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 몇가지 금속-Dithiocarbamate 킬레이트의 용리거동 및 동시분석에 관한 연구)

  • Dai Woon Lee;Yun Je Kim;Hyun Chul Kim;Won Lee
    • Journal of the Korean Chemical Society
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    • v.32 no.3
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    • pp.211-226
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    • 1988
  • Liquid chromatographic behavior of several metal ions in dithiocarbamate(DTC) chelates were investigated by reversed phase high performance liquid chromatography on Novapak $C_{18}$ and ${\mu}$-Bondapak $C_{18}$ columns. The optimum conditions for the separation of DTC-metal chelate were examined with respect to the pH, shaking time, flow rate, extraction solvent, and mobile phase strength. The metal ions in mixtures at trace level, chelated with some dithiocarbamate derivatives were separated successfully on Novapak $C_{18}$ column using acetonitrile/methanol/water or acetonitril/water mixtures as mobile phases. It was found that all DTC metal chelates studied were eluted in an acceptable range of capacity factor values ($0{\leqq}log\;k'{\leqq}1$). Although several foreign metal ions were coexisted, high recovery and good precision were attained ; 97.0-106.7 % for the recovery and 0.98-3.41% for the coefficient of variation. Under the optimum analytical conditions, trace metal ions in the composite water samples were determined sucessfully with in relative error of about {\pm}$6.7 %.

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Determination of Boron by Ion Pair Liquid Chromatography with Chromotropic Acid (Chromotropic Acid를 착화제로 이용한 이온쌍 액체 크로마토그래피에 의한 붕소의 분리와 정량)

  • Yun, Young Ja;Yu, Gu Yong
    • Journal of the Korean Chemical Society
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    • v.39 no.4
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    • pp.288-293
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    • 1995
  • The separation and determination of boron with chromotropic acid (1,8-Dihydroxynaphthalene-3,6-disulfonic acid) as a complex agent has been studied using ion pair liquid chromatography. The use of tetrabutylammonium bromide added as an ion pair reagent to mobile phase (MeOH 61%, phosphate buffer 39% pH=8.5) allowed good separation of boron-chromotrophic acid complex anion and chromotrophic acid on poly(styrene-divinylbenzene) based reversed phase column (PRP-1, 15 $cm{\times}4.6$ mm i.d.). The complex formation between boric acid and chromotrophic acid was enhanced in the presence of 0.1 M tetrabutylammonium bromide, resulting in high sensitivity. The linear calibration was achieved over the boron concentration range of 0.5∼1000 ${\mu}g/L.$ The detection limit was 0.5 ${\mu}g/L$ (S/N=2). The proposed method was applied to the determination of boron in commercially available chemicals, $Na_2SO_4$, NaOH, KCl.

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Empirical Equation for Resolution if Ibuprofen Enantiomers by Chiral High-Performance Liquid Chromatography (키랄 고성능 액체 크로마토그래피를 이용하 이부프로펜의 분리도에 관한 실험식)

  • 여미순;노경호
    • KSBB Journal
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    • v.18 no.4
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    • pp.261-265
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    • 2003
  • Ibuprofen was analyzed by chiral high performance liquid chromatography. Retention behaviours of the standard mixtures of ibuprofen were investigated to obtain their acceptable resolution. A chromatographic column (3.9 ${\times}$ 300 mm) was packed by Kromasil CHI-TBB packings (10 $\mu\textrm{m}$) and n-hexane was used as a mobile phase with 0.1% acetic acid and tert-butyl methyl ether. Isocratic elution of ibuprofen at 1.0 $m\ell$/min was performed by changing the mobile phase compositions. The experimental variables affecting the resolution were the compositions of mobile phase and chemical buffer (n-hexane and tert-butyl methyl ether). The resolution between the enantiomers were correlated into the several types of empirical equations including linear form, and their agreements between experimental data and calculated values were examined by the regression coefficient.

Bitter Peptides Derived from ${\alpha}_{s1}-and\;{\beta}-Casein$ Digested with Alkaline Protease from Bacillus subtilis (Bacillus subtilis의 염기성 프로테아제로 분해된 ${\alpha}_{s1}$- 및 ${\beta}$-카세인에서 분리된 쓴 맛 펩타이드)

  • Sohn, Kyung-Hyun;Lee, Hyong-Joo
    • Korean Journal of Food Science and Technology
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    • v.20 no.5
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    • pp.659-665
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    • 1988
  • The ${\alpha}_{s1}$-and ${\beta}$-casein were purified by DEAE-cellulose chromatography and digested with alkaline protease from Bacillus subtilis. Bitter fractions from the hydrolyzates were isolated using n-butanol extraction, Sephadex G-25 gel chromatography, and high performance liquid chromatography. Peptide mixtures were separated by reverse-phase octadecyl silica column with linear gradient of 0-80% acetonitrile containing 0.1% trifluoroacetic acid. Major peaks were combined from replicate chromatographies and the bitterness of each peak was evaluated. The bitter-tasting peaks were rechromatograpied until isolated peaks were obtained. Three different bitter peptides(BP-I, BP-II, BP-III) were obtained from the ${\alpha}_{s1}$-casein hydrolyzate. BP-I was eluted at 34% acetonitrile and BP-II, 35%, BP-III, 26%, respectively. Two bitter peptides(BP-IV, BP-V) were isolated from the ${\beta}-casein$ hydrolyzate: BP-IV was eluted at 40% acetonitrile and BP-V, 42%. BP-V was the most hydrophobic peptide in the five bitter peptides. However, BP-I and BP-II tasted more bitter than BP-IV and BP-V.

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Determination of allyl isothiocyanate, capsaicin and dihydrocapsaicin in pungent liquid samples (자극성 액체시료 중 Allyl Isothiocyanate, Capsaicin and Dihydrocapsaicin 정량에 관한 연구)

  • Kim, Sang-Soo;Choi, Jong-Moon
    • Analytical Science and Technology
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    • v.26 no.1
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    • pp.73-79
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    • 2013
  • The allyl isothiocyanate, capsaicin and dihydrocapsaicin as main components in self defense sprays were determined by gas chromatography-mass spectrometer (GC-MS). Although self defense spray was used to protect by myself, a social problem could be caused by the hazard of spray chemical due to use pungent liquid. To identify this, the pH of pungent liquid solutions, solubility to detergents, the existence of other materials and the types and amounts of pungent material in spray chemicals were investigated in this work. Finally, the amounts of allyl isothiocyanate, capsaicin and dihydrocapsaicin as pungent materials in them were determined by GC-MS. The pH of chemicals were about 5.7 as weak acid, the detergents can emulsify them with water well. And they did not contain fluorescent materials and hazard organic solvents. The pungent components in three real samples were only allyl isothiocyanate [47,600 mg/kg (47.6%)] in one sample, and mixtures with capsaicin [228 mg/kg~368 mg/kg (1.14%~1.84%)] and dihydrocapsaicin [224 mg/kg~414 mg/kg (1.12%~2.07%)] in the others, respectively.

Chromatographic Separation of Hydrogen Isotopes by Deactivated Alumina Stationary Phase (비활성 알루미나 고정상을 이용한 수소동위원소의 크로마토그래피 분리)

  • Kim, Kwang Rag;Lee, Sung Ho;Kang, Hee Suk;Chung, Hongsuk;Sung, Ki Woung
    • Applied Chemistry for Engineering
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    • v.9 no.1
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    • pp.121-128
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    • 1998
  • In fields of operating or handling a hydrogen isotope facility, and of the technology for nuclear fusion source management, gas chromatography has been used as one of the practical techniques lot separation and enrichment of hydrogen isotopic gases including tritium. Chromatographic separation experiments of the hydrogen isotope mixture (hydrogen, deuterium and tritium) were carried out by use of a commercially available gas chromatograph. An aliquot of gas sample was injected by a specially designed vacuum sampler into the stream of inert carrier gas which went through the separation column under liquid nitrogen temperature. The complete separation of hydrogen isotopic molecules was observed with an alumina adsorbent partially deactivated by coating with 10% manganese chlorine. In addition, fairly good separation conditions were obtained without any appearance of nuclear spin isomers with shorter retention time, which would be available for the practical applications of the hydrogen isotope separation and enrichment.

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Studies on the Simultaneous Analysis of Organochlorine Pesticide Residues by Gas-Liquid Chromatography (II). Determination of Pesticides by GLC (기체-액체 크로마토그래피에 의한 잔류 유기염소제 농약들의 동시 분석에 관한 연구 (제2보). GLC에 의한 농약의 정량)

  • 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.503-509
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    • 1985
  • Sixteen organochlorine pesticides extracted out from the crops and cleaned by solvent-solvent partitioning and Florisil column chromatography were determined by gas-liquid chromatography. The majority of the pesticides were well separated by being eluted through 5% QF-1 column and some of them through 3% OV-17 column and 2.596 DC-200/2.5% QF-1 column, and the eluted pesticides were detected by $^{63}Ni$ electron capture detector. The linear calibration curves were obtained for the most of pesticides while some curves were slightly deviated from the linearity. In the determination of 16 pesticides added to thirteen kinds of crops, the recoveries were showed over 85% for the most cases and the relative standard deviations of 5 analyses were less than 12.1%. The results were within the criteria of the AOAC method.

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