• Title/Summary/Keyword: eluent

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Simultaneous Determination of Chlorogenic Acid and Linarin in Chrysanthemum Sibiricum Fisher by Reversed-Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 구절초 중 Chlorogenic Acids와 Linarin의 동시 정량분석)

  • Kim, Taek-Jae;Lee, Tae-Ryong;Park, Ho-Koon
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.720-724
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    • 1991
  • Simultaneous determination of chloragenic acid (CA), 3,4-o-dicafeoyl quinic acid(3,4-DCQA), 4,5-o-dicaffeoyl quinic acid (4,5-DCQA) and linarin in Chrysanthemum sibiricum Fisher was newly established by a reversed-phase high performance liquid chromatography (HPLC). Sample was extracted with 20 ml methanol for 4 hrs. The extract was cleaned up by using Sep-Pak $C_18$ cartridge and 4 ml methanol-$H_2$O(1 : 1) as eluent. Their determination was performed by means of RP-HPLC with Bondapak $C_18$ column (30 cm ${\times}$ 3.9 mm i.d., 10 ${\mu}m$ and gradient elution mode as methanol-5 mM $H_3PO_4$ solution (30 : 70). The established method was applied to various samples purchased. As a result, their content ranges showed to be 0.35~0.55% for CA, 0.46~0.76% for 3,5-DCQA, 0.077~0.23% for 4,5-DCQA and 0.16~2.72% for linarin, respectively.

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An Improved Method for Multiresidue Analysis of Pesticides in Lettuce, Chinese Cabbage and Green Pepper by Gas Chromatography

  • Hong, Yong-Soon;Park, Hee-Won;Choi, Hoon;Moon, Joon-Kwan;Kim, Min-Jeong;Kim, Jang-Eok;Lee, Young-Deuk;Oh, Chang-Hwan;Kim, Jeong-Han
    • Korean Journal of Environmental Agriculture
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    • v.23 no.3
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    • pp.158-169
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    • 2004
  • For the improvement of gas chromatographic analysis of multiple pesticide residues in green pepper, lettuce and Chinese cabbage, multiresidue test mixtures (MRTMs) of 10 groups (ECD 5 groups and NPD 5 groups) and a recovery test mixture (RTM) of 18 compounds (11 compounds for ECD and 7 compounds for NPD) were established based on retention time and response to relevant detectors. A new extraction solvent (acetone: acetonitrile=1 : 9) and a clean up eluent (hexane: dichloromethane : acetonitile = 50 : 48.5 : 1.5) for solid-phase extraction (SPE) cartridge were selected to test two types of multiresidue methods (MRM I and MRM II). MRM II provided high recovery better than MRM I when RTM was tested Recovery experiment with MRTMs which was conducted using MRM II resulted in that more than seventy percents of compounds were recovered in the range of $50{\sim}140%$, while 9% of compounds were over 140% of recovery and only $7{\sim}8$ compounds failed to detect. MRM II, an improved method, could be employed for screening residues of 190 pesticides in those vegetables.

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

  • Choi, Il-Hwan;Jung, Yu-Jin
    • Journal of Korean Society on Water Environment
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    • v.24 no.6
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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.

Effect of Temperature and Eluent Composition on the Separation of Ketoprofen and Ibuprofen Racemates in Kromasil HPLC Column (Kromasil HPLC 칼럼에서 온도와 이동상 조성비에 따른 Ketoprofen과 Ibuprofen 라세미체의 분리특성)

  • Park, Moon-Bae;Kim, In Ho
    • Korean Chemical Engineering Research
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    • v.47 no.1
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    • pp.54-58
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    • 2009
  • Ketoprofen and ibuprofen are non-steroid anti-inflammatory drug(NSAID) that have analgesic and antipyretic properties. (S)-ketoprofen and (S)-ibuprofen have pharmacological activity, while (R)-ketoprofen and (R)-ibuprofen are either inactive or have side effect. The chiral separation of racemic ketoprofen and ibuprofen enantiomers was carried out by using a Kromasil HPLC column. Some chromatographic parameters (selectivity, resolution, number of theoretical plates and ${\Delta}H$) are calculated under different mobile phase compositions of hexane/t-BME/acetic acid and temperatures. The selectivity, resolution and number of theoretical plates were observed high at $25^{\circ}C$ and the composition of hexane/t-BME/acetic acid (80/20/0.1).

A Study on the Purification Process of Methyl Fructoside by Liquid Chromatography (액체 크로마토그래피에 의한 메틸프룩토시드의 분리공정 연구)

  • 허주형;유인상김해성
    • KSBB Journal
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    • v.11 no.5
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    • pp.529-535
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    • 1996
  • Methyl frucloside was purified from the aqueous sugar/methyl fructoside solution by liquid chromatography using Amberlite IRA-900, strong anion-exchange resin. The optimum operating conditions, resolution and productivity of methyl fructoside were discussed to evaluate the practical feasibility of the proposed chromatographic separation process of methyl fructoside which is useful as a new starting material for sugar ester synthesis. The linear chromatography model with HETP was well applied to the chromatographic separation process of methyl fructoside and the theoretical solution successfully predicted the elution chromatogram of methyl fructoside and sucrose at different superficial linear velocity of eluent for rectangular feed with different loading volume of packed bed. The optimum operating conditions were found to be 75% with the loading volume of packed bed at 1.13 cm/min of the superficial linear velocity at $60^{\circ}C$, and gave the productivity of methyl fructoside of 7 mg/g-resin/h with the resolution of 1.1.

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Enrichment of Lithium Isotope by an Ion Exchange Resin Containing Azacrown Ether (아자크라운 에터를 포함한 이온교환수지에 의한 리튬 동위원소의 농축)

  • Kim, Dong Won;Chung, Yongsoon;Choi, Ki Young;Lee, Yong-Ill;Jeong, Young Kyu;Jang, Young Hun
    • Analytical Science and Technology
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    • v.10 no.6
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    • pp.403-407
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    • 1997
  • Separation factor for $^6Li$ and $^7Li$ have been determined using ion exchange resin having 1,7,13-trioxa-4,10,16-triazacyclooctadecane($N_3O_3$) as an anchor group. The lighter isotope, $^6Li$ is concentrated in the solution phase, while the heavior isotope, $^7Li$ is enriched in the resin phase. By Ccolumnl chromatography[0.9cm(I.D)${\times}$20cm(height)] using 2.0M ammonium chloride solution as an eluent, single separation factor, ${\alpha}$, 1.009. i.e.$(^7Li/^6Li)_{resin}$/$(^7Li/^6Li)_{solution}$ was obtained by the Glueckauf theory from the elution curve and isotope ratios.

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Separation Characteristics of Ibuprofen in Kromasil HPLC Column (Kromasil HPLC 칼럼을 이용한 Ibuprofen의 분리특성 연구)

  • Park Joon Sub;Kim Byung Lip;Yoon Tae Ho;Kim In Ho
    • KSBB Journal
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    • v.20 no.3
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    • pp.244-249
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    • 2005
  • Chiral separation of racemic ibuprofen was achieved on a Kromasil KR100-5CHI-TBB column. Some chromatographic parameters (resolution, number of theoretical plates, HETP, capacity factor) are calculated under different separation conditions such as change of mobile phase compositions (hexane / t-BME : 85 / 15, 75 / 15, 65 / 35, 55 /45) as well as acetic acid concentrations for adjusting pH (0.1 to 1 $v/v\%$). Flow rate versus number of theoretical plates and HETP were compared to evaluate column efficiency. To determine the adsorption isotherms, PIM (Pulsed Input Method) was carried out. At concentrations of racemic ibuprofen between 0.1 and 0.3 mg/ml, S- and R-ibuprofen have the same retention time of 4.48 and 5.81 min. Ibuprofen isotherms show a linear form under concentrations of 0.3 mg/ml with eluent (hexane / t-BME = 55 / 45).

Separation and Recovery of Rare Earths by Ion Exchange Chromatography (이온교환 크로마토그래피에 의한 희토류 원소의 분리와 회수)

  • Cha, Ki Won;Park, Kwang Won;Hong, Sung Wook
    • Journal of the Korean Chemical Society
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    • v.41 no.11
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    • pp.612-638
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    • 1997
  • The methods of separation and recovery of rare earth elements in monazite sand have been studied by the ion exchange chromatography. Both of cation and anion exchange resin were used as ion exchange resins and the solutions of EDTA, DTPA, IMDA and Ln-EDTA were used as eluents. The H+, Zn2+, Fe3+, Al3+, Cu2+, and NH4+ forms of cation exchange resin were used as retaining ions. Ln-EDTA solution was loaded on the EDTA form of anion exchange resin and separated. The Ln-EDTA solution was also used as an eluent for a selective separation of one element from the rare earth mixture solution. The size effects of resin column, the elution mechanism for the various elution types and the separation of a large amount of rare earths were studied.

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Linear Solvation Energy Comparison Study in Normal Phase Liquid Chromatography Ⅰ (정상 액체크로마토그래피에서의 선형 용매화에너지 비교법 연구 Ⅰ)

  • Choe, Jang Deok;Jeong, Won Jo
    • Journal of the Korean Chemical Society
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    • v.38 no.3
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    • pp.221-223
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    • 1994
  • We tried to apply the linear solvation energy comparison method to solute retention in normal phase liquid chromatography. Correlation coefficients of regression of lnk' collected in a fixed eluent against solute polarity indices have proven to be lower than those obtained from reversed phase liquid chromatography data. This event can be attributed to complexity of solute retention process in normal phase liquid chromatography. We concluded from the regression results that each specific polarity of the stationary phase is greater than that of the mobile phase and that the difference in each polarity between the stationary phase and the mobile phase decreases as the volume fraction(${\phi}$) of the more polar solvent in the mobile phase increases. Correlations of lnk' of a single solute against solvent polarity indices have proven to be meaningless owing to covariance among the solvent polarity indices. Instead, a good linear relationship between lnk' and solvent ${\pi}^*$ was observed, and its linearity is better than that between lnk' and ${\phi}$.

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Study on the Separation and Determination of Pure Rare Earth Oxides by Anion Exchange Resin (음이온 교환수지에 의한 고순도 희토류산화물의 분리 및 정량에 관한 연구)

  • Cha, Gi Won;Ham, Yun Beom
    • Journal of the Korean Chemical Society
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    • v.34 no.6
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    • pp.606-615
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    • 1990
  • The purity of CeO$_2$, Sm$_2$O$^{3+}$ and La2O$^{3+}$ have been determinated by separating the impurity of rare earth-elements in those oxides with anion exchange resin and measuring the absorbance of the separated element with MTB. 1 ml of the mixture solution containing each 1 mg/ml of Y$^{3+}$, Yb$^{3+}$, Eu$^{3+}$, Sm$^{3+}$, Nd$^{3+}$, Pr$^{3+}$, Ce$^{4+}$and La$^{3+}$ is loaded in top layer of anion exchange resin column, Amberlite CG400 and separated with the mixture solution of the various concentration of methyl alcohol and nitric acid as an eluent. Using the result, the impure rare earth elements in pure CeO$_2$, Sm$_2$O$^{3+}$ and La$_2$O$^{3+}$ are determinated.

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