• Title/Summary/Keyword: Reversed phase chromatography

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Reversed-Phase Ion-Interaction Chromatography of Aromatic Sulfonic and Carboxylic Acids (방향족 슬폰산 및 카르복시산의 역상 이온-상호작용 크로마토그래피)

  • Kang Sam-Woo;Oh Hae-Beom;Lee Seung-Seok
    • Journal of the Korean Chemical Society
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    • v.32 no.2
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    • pp.113-121
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    • 1988
  • The retention mechanism and separation of various aromatic sulfonic and carboxylic acids on reversed-phase liquid chromatographic column were studied in the mobile phase containing dodecyltrimethylammonium bromide (DTAB). The retention mechanism was found to be followed the ion-interaction model where the DTAB occupies a primary layer at the stationary phase while the sample anions and other co-anions in the system compete for forming the secondary layer. The capacity factors of samples were influenced by the several factors such as pH, concentration of various organic solvents, co-anions in the mobile phase and functional groups in sample molecules. Some mixtures of organic samples were attempted to separate under optimum condition.

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Reversed-Phase Liquid Chromatographic Separation of Metal Ions by Chelate Formation with 1-(2-Pyridylazo)-2-Naphthol (역상 액체크로마토그래피에 의한 1-(2-Pyridylazo)-2-Naphthol과 킬레이트를 형성하는 금속이온의 분리)

  • Kang, Sam Woo;Park, Sun Ja
    • Journal of the Korean Chemical Society
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    • v.42 no.2
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    • pp.197-202
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    • 1998
  • 1-(2-Pyridylazo)-2-Naphthol (PAN) has been widely used as a spectrophotometric reagent and metallochromic indicator for many metal ions. In this work, the chelate reagent of PAN was used as mobile phase additive for the separation of metal ions by reversed phase chromatography. Metal ions could be detected by monitoring the effluent at 570 nm with spectrophotometric detector. In order to investigate retention behaviors of the metal ions, the chromatograms and capacity factors were obtained as the variation of pH, ionic strength and composition of organic modifier in mobile phase. Under the obtained optimum conditions, the mixtures of Fe(III), Ni(II), Cu(II), Zn(II) and Co(II) could be separated successfully and the calibration curves under the recommended conditions showed an excellent linearity. The detection limits(S/N) were feasible at the nanogram level.

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Studies on The Elution Behavior of Ni(II)-${\alpha}$-isonitroso-${\beta}$-diketone Imine Chelates in Reversed-Phase Liquid Chromatography

  • Lee, Won;Kim, In-Whan;Kim, Mi-Kyoung;Kim, Yong-Jun;Jung, Hae-Rim;No, Kyoung-Tai;Kim, Su-Yeon
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.519-527
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    • 1995
  • The retention mechanism of Ni(II)-${\alpha}$-isonitroso-${\beta}$-diketone imine chelates in reversed-phase HPLC has been studied by examining the effect of temperature, mobile phase composition in acetonitrile-water mixture, and molecular structure on retention. The empirical retention equation was investigated to evaluate the properties of S (hydrophilic index). The value of the S index of the Ni(II) chelates decrease with the increasing column temperature and a linear relationship between S and log $k{_w}^{\prime}$ has been found. The results showed that the S index is influenced by the interaction between Ni(II) chelates and mobile phase. Molecular properties, van der Waals molar volume, polarizability and dipole moment, of the Ni(II) chelates were calculated by Cerius 2 program and the calculations were performed at Universal Force Field (UFF) model. The S value and log $k{_w}^{\prime}$ increase with decreasing the dipole moment of Ni(II) chelates.

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Simultaneous Separation Analysis of Some Metal Ions in Piperidinedothiocarbamate Chelates by Reversed-Phase Liquid Chromatography (역상 액체 크로마토그래피에 의한 몇가지 금속 이온들의 Piperidinedithiocarbamate 킬레이트 동시분리분석)

  • Lee, Won;Bahng, Seung-Hoon;Kim, Mi-Kyoung
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.27-33
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    • 2000
  • Simultaneous separation and analysis of Ni(II), Pd(II), Co(II), Cu(II) and Hg(II) in peperidinedithiocarbamate (PDTC) chelates were investigated by reversed phase liquid chromatography. The optimum conditions for the separation of PDTC metal chelates were examined with respect to the pH, extraction solvent, and mobile phase strength on Novapak $C_{18}$ column using methanol/water mixture as mobile phase. All metal PDTC chelates were eluted in an acceptable range of capacity factor value ($0{\leq}log\;k^{\prime}{\leq}1$). The linear calibration curves were obtained in the concentration range of $0{\sim}1.2{\mu}g/mL$ for five metal ions, and also good precision in the range of 1.96~3.41% RSD was obseved. Under the optimum conditions, trace metat ions in the composite water sample were successfully separated and determined with relative error of ${\pm}2.0%$.

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Improved Calibration for the Analysis of Emerging Contaminants in Wastewater Using Ultra High Performance Liquid Chromatography and Time-of-Flight Mass Spectrometry

  • Pellinen, Jukka;Lepisto, Riikka-Juulia;Savolainen, Santeri
    • Mass Spectrometry Letters
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    • v.9 no.3
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    • pp.77-80
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    • 2018
  • The focus of this paper is to present techniques to overcome certain difficulties in quantitative analysis with a time-of-flight mass spectrometer (TOF-MS). The method is based on conventional solid-phase extraction, followed by reversed-phase ultra high performance liquid chromatography of the extract, and mass spectrometric analysis. The target compounds included atenolol, atrazine, caffeine, carbamazepine, diclofenac, estrone, ibuprofen, naproxen, simazine, sucralose, sulfamethoxazole, and triclosan. The matrix effects caused by high concentrations of organic compounds in wastewater are especially significant in electrospray ionization mass spectroscopy. Internal-standard calibration with isotopically labeled standards corrects the results for many matrix effects, but some peculiarities were observed. The problems encountered in quantitation of carbamazepine and triclosan, due to nonlinear calibration were solved by changing the internal standard and using a narrower mass window. With simazine, the use of a quadratic calibration curve was the best solution.

Recent Developments in High-performance Liquid Chromatography of Lipids

  • Christie, William W.
    • Journal of the Korean Applied Science and Technology
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    • v.10 no.1
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    • pp.1-8
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    • 1993
  • The possibilities for HPLC analysis of lipids have been revolutionised by the availability of evaporative light-scattering detectors, with which the response is independent of the nature of the mobile phase and does not depend On the presence of specific chromophores in the lipids. It was thus possible to develop an HPLC procedure, involving ternary gradient elution, for separating all the lipid classes in animal tissues in a single step. Although reversed-phase HPLC has been widely used for the analysis of molecular species of lipids, sliver ion chromatography can be a valuable alternative. For example, a stable silver ion column for HPLC was developed which permitted resolution of molecular species of triacylglycerols, even from such complex samples as fish oils, again With light-scattering detection and gradient elution. The capacity for HPLC resolution of diastereomeric diacyl-sn-glycerol derivatives, prepared from triacylglycerols. has lead to a new simple method for stereospecific analysis of the latter.

Determination of Byakangelicin in Angelicae dahuricae Radix by High Performance Liquid Chromatography (고속액체크로마토그라피에 의한 백지근 중 Byakangelicin의 정량)

  • Shin, Kuk-Hyun;Kang, Sam-Sik;Chi, Hyung-Joon
    • Korean Journal of Pharmacognosy
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    • v.21 no.3
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    • pp.239-241
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    • 1990
  • A new method for quantitative determination of byakangelicin in Angelicae dahuricae Radix by high performance liquid chromatography was established. A reversed-phase system with a ${\mu}Bondapak$ $C_{18}$ column using THF : dioxane : MeOH : HAc : 5% $H_3PO_4$ : $H_2O$=72.5 : 62.5 : 25 : 10 : 1 : 329 as a mobile phase was developed. Byakangelicin together with ter-O-byakangelicin and oxypeucedanin methanolate, and isooxypeucedanin as an internal reference were detected at 350 nm and the analysis was successfully carried out within 30 min.

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Determination of p-Methoxycinnamic Acid in Scrophulariae Radix by High Performance Liquid Chromatography (고속액체크로마토그라피에 의한 현삼근(玄蔘根) 중 p-Methoxycinnamic acid의 정량)

  • Lee, Sang-Hyun;Chi, Hyung-Joon;Shin, Kuk-Hyun
    • Korean Journal of Pharmacognosy
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    • v.30 no.3
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    • pp.328-331
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    • 1999
  • A new method for quantitative determination of p-methoxycinnamic acid in Scrophulariae radix by high performance liquid chromatography was established. A reversed-phase system with SPHERI-5 RP-18 5 micron $(250\;{\times}\;4.6\;mm)$ column using TFA (0.05%) and acetonitrile as a mobile phase was developed. p-Methoxycinnamic acid and N-(p-methoxycinnamoyl)-p-aminophenol as an internal reference were detected at 310 nm and the analysis was successfully carried out within 50 min.

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Determination of Icariin in Epimedii Herba by High Performance Liquid Chromatography (고속액체크로마토그라피에 의한 음양곽 중 Icariin의 정량)

  • Shin, Kuk-Hyun;Kang, Sam-Sik;Chung, Sun-Gan;Cho, Eui-Hwan
    • Korean Journal of Pharmacognosy
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    • v.20 no.1
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    • pp.21-24
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    • 1989
  • A new method for quantitative determination of icariin in Epimedii Herba by high performance liquid chromatography was established. A reversed-phase system with $a\;{\mu}Bondapak\;C_{18}$ column using methanol in water(15% to 70%, gradient elution) as a mobile phase was developed. Icariin and spinosin as an internal reference were detected at 350 nm and the analysis was successfully carried out within 30 min.

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Determination of Catecholamines and Their Metabolites in Rat Brain by High Performance Liquid Chromatography with Electrochemical Detector (HPLC-ECD에 의한 흰쥐 뇌 부위별 Catecholamine 및 대사산물의 신속정량법)

  • Ro, Ihl-Hyeob
    • YAKHAK HOEJI
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    • v.32 no.1
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    • pp.50-54
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    • 1988
  • A simple and sensitive method was studied for the simultaneous determination of catecholamine, indoleamine and their related metabolites by high performance liquid chromatography with electrochemical detector. Norepinephrine, dopamine, serotonin and their metabolites of 3,4-dihydroxyphenylacetic acid, homovanillic acid, 5-indoleacetic acid were resolved from rat brain tissue homogenates by separation on reversed phase $C_{18}$ column with mobile phase consisting of monochloroacetate buffer (pH2.47), 1.42mM sodium octyl sulfonate and 7% acetonitrile. Both catechols and indoles can be eluted in 15min. The sensitivities of this method are sufficient for determination of at least 100 pg of neurochemical amines in brain samples, for example, frontal cortex, olfactory bulb, striatum, septum, hippocampus, thalamus, hypothalamus, medulla & pons and cerebellum. The highest level of dopamine was observed in striatum whereas norepinephrine and serotonin were in hypothalamus.

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