• Title/Summary/Keyword: Reversed phase liquid chromatography

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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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Validation of Analysis Methods of Decursin and Decursin angelate from Angelicae gigantis Radix by Reversed-phase Liquid Chromatography

  • Ze, Keum-Ryon;Park, Sang-Young;Cho, Chang-Hee;Sung, Rak-Sun;Lee, Jong-Pil;Park, Ju-Young;Cho, So-Yean;Jin, Zhexiong;Kim, Jun-Hyuk
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.288.1-288.1
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    • 2003
  • The determination method of decursin and decursin angelate from Angelicae gigantis Radix, an important crude drug in oriental medicine, was developed and validated by a reverse-phase liquid chromatography. The decursin and decursin angelate, the structural isomer aspyranocoumarin each other, are the main organic constituents in Angelicae gigantis Radix. (omitted)

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Thermodynamic Properties of the Solute Transfer from the Aqueous Acetonitrile Mobile Phase to the Stationary Phase Monitored by HPLC

  • Jeong, Won Jo;Kim, Ji Yeon;Gu, Yun Mo
    • Bulletin of the Korean Chemical Society
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    • v.21 no.1
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    • pp.105-109
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    • 2000
  • High-performance liquid chromatography is suitable for getting thermodynamic information about solute-solvent interactions. We used a squalane impregnated $C_{18}$ phase as a presumably bulk-like stationary phase to secure a simple partition mechanism for solute retention in reversed phase liquid chromatographic system. We measured retention data of some selected solutes (benzene, toluene, ethylbenzene, propylbenzene, butylbenzene, phenol, benzylalcohol, phenethylalcohol, benzylacetone, acetophenone, benzonitrile, benzylcyanide) at 25, 30, 35, 40, 45, and 50 $^{\circ}C$ in 30/70, 40/60, 50/50, 60/40 and 70/30 (v/v%) acetonitrile/water eluents. The van't Hoff plots were nicely linear, thus we calculated dependable thermodynamic values such as enthalpies and entropies of solute transfer from the mobile phase to the stationary phase based on more than four retention measurements on different days (or weeks). We found that the cavity formation effect was the major factor in solute distribution between the mobile and stationary phases in the system studied here. Our data were com-pared with some relevant literature data.

A Study on the Retention Behavior of Co(II)-Dithiocarbamate Chelates in Reversed Phase-High Performance Liquid Chromatography (역상 액체크로마토그래피에서 Co(II)-Dithiocarbamate 킬레이트의 머무름 거동에 관한 연구)

  • Lee, Won;Kim, Eun-Kyung;Ann, Hye-Sook;Lee, Jung-Han
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.387-396
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    • 1999
  • The retention behavior of Cot(II)-dithiocarbamate(DTC) chelates in reversed phase high performance liquid chromatography was investigated. Enthalpy and entropy of chelates transfer from the mobile phase to the stationary phase were calculated from retention data using van't Hoff plots. The dependence of In k' on enthalpy was decreased with increasing organic solvent ratio on the mobile phase. The compensation temperatures(${\beta}$) calculated from the slope of $-{\Delta}H^0$ vs In k' were in the range of 756.3-888.5 K. From these results. it was found that the retention mechanism of DTC chelates was invariant under the various temperatures and was largely affected by the solvophobie effect. Liniear relationship between S index and log k' in emprical retention equation, $log\;k^{\prime}=log\;{k_w}^{\prime}-S_{\varphi}$ showed that S index was influenced mainly by the interaction between DTC chelates and the mobile phase.

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Chiral separation of $\beta$-agonists after derivatization with a new chiral derivatization agent, GATC

  • Min, Kyeong-Il;Ko, Mi-Young;Kim, Kyeong-Ho
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.275.2-276
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    • 2003
  • Several ${\beta}$-agonists were investigated for the possible separation of the enantiomers by reversed-phase high-performance liquid chromatography after derivatization with a new chiral derivatization agent, GATC. The derivatization proceeded quantitatively within 1 h at room temperature. The corresponding diastereomers were well resolved an ODS column with acetonitrile-acetate buffers a mobile phase and monitored at UV 254nm. (omitted)

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Identification and Quantitative Analysis of Flavonol Glycosides from Ginkgo biloba Leaves by High Performance Liquid Chromatography (고속액체크로마토그라피에 의한 은행잎중 Flavonoid Glycoside의 확인 및 정량)

  • Kang, Sam-Sik;Kim, Ju-Sun;Kwak, Wie-Jong;Kim, Ki-Hyup
    • Korean Journal of Pharmacognosy
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    • v.21 no.2
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    • pp.148-152
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    • 1990
  • Seven flavonol glycosides from the EtOAc fraction of Ginkgo biloba leaves were identified by high performance liquid chromatography. Separation by reversed phase chromatography on $Lichrosorb^{\circledR}$ RP-18 column was achieved by isocratic elution. The content of the major acylated flavonol glycoside, kaempferol 3-0-[$6'-O-{p}-coumaroyl-{\beta}-_D-glucosyl(1{\rightarrow}2)-{\alpha}-_L-rhamnoside$] was about 8.0% and 0.55% for EtOAc fraction and MeOH extract, respectively.

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Separation and Elution Behavior of Some Iron(Ⅲ)porphyrin Complexes by Reversed-Phase Liquid Chromatography (역상 액체 크로마토그래피에 의한 Iron(Ⅲ)porphyrin 착화합물들의 분리 및 용리거동에 관한 연구)

  • Chang Hee Kang;In Whan Kim;Won Lee
    • Journal of the Korean Chemical Society
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    • v.37 no.12
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    • pp.1035-1046
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    • 1993
  • Some iron(III)porphyrin complexes were prepared, and identified by the spectroscopic methods. Elution behavior of iron(III)porphyrin complexes was investigated by reversed-phase HPLC. The optimum conditions for the separation of iron(III)porphyrin complexes were examined with respect to flow rate and mobile phase strength. These complexes were successfully separated on NOVA-PAK $C_{18}$ column using methanol / water(95/5) for $[T_pCF_3PP)Fe(R)]$ and methanol / water (98/2) for $[(P)Fe(C_6F_5)]$ as a mobile phase. It was found that these complexes were largely eluted in an acceptable range of capacity factor value ($0{\leq}logk'{\leq}1$). The dependence of the capacity factor (k') on the volume fraction of water in the binary mobile phase as well as the dependence of k' on the liquid-liquid extraction distribution ratio$(D_c)$ in methanol-water / n-pentadecane extraction system showed a good linearity. It means that the retention of iron(III)porphyrin complexes on NOVA-PAK $C_{18}$ column is largely due to the solvophobic effect. Also, there was a good linear dependence of the capacity factor(k') on the column temperature and enthalpy calculated by van't Hoff plot. From these results, it was confirmed that the retention mechanism of iron(III)porphyrin complexes in reversed-phase liquid chromatography was invariant under the condition of various temperature, and the solvophobic binding process exhibited isoequilibrium behavior.

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Separation of Functionalized Heterocyclic Compounds by High Performance Liquid Chromatography(I) (고성능 액체 크로마토그래피에 의한 기능성 헤테로고리화합물의 분리(I))

  • Lee, Kwang-PilI;Cho, Yun Jin;Lee, Young Cheol
    • Analytical Science and Technology
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    • v.10 no.6
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    • pp.408-417
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    • 1997
  • Normal phase or reversed phase liquid chromatographic separation of some structural isomers of functionalized heterocyclic compounds has been carried out by using several different columns and various mobile phases. The optimal experimental conditions for separation of structural isomers were found on a ternary solvent system including alcohol as a modifier. This polar modifier is preferentially adsorbed onto strong adsorption site, leaving a more uniform population of weaker site that then serve to retain the sample. This 'deactivation' of the adsorbent leads to a number of improvements in subsequent separations. The optimal mobile phase system of separation were found on normal phase on structural isomers. Retention mechanism of normal phase system was also studied depending on adsorption strength between solute and stationary phase of column. However, retention factors of reversed phase system were found on hydrophobic interaction with solvophobic effect.

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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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