• Title/Summary/Keyword: reversed-phase HPLC

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A Study on the Elution Behavior of some Metal-N-Alkylisonitrosoacetylacetone imine Chelates by Reversed Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 몇 가지 금속-N-Alkylisonitrosoacetylacetone imine 킬레이트의 용리거동에 관한 연구)

  • Kim, Yong Jun;Kewon, Ji Hae;Lee, Won
    • Analytical Science and Technology
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    • v.5 no.1
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    • pp.63-71
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    • 1992
  • Liquid chromatographic behavior of Pd(II), Ni(II) and Co(III) in N-Alkylisonitrosoacetylacetone imine(HIAA-NR) chelates was investigated by reversed phase high perfomance liquid chromatography. The optimum conditions for the separation of IAA-NR-metal chelates were examined respect to the flow rate and mobile phase strength. The metal-N-Alkylisonitrosoacetylacetone imine chelates in solution were successfully separated on Novapak $C_{18}$ column using acetonitrile/water mixture as mobile phase. The elution order of chelates is methyl>ethyl>propyl>butyl as N-alkyl group for ligand is varied. It was found that all IAA-NR-metal chelates were eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of log k' on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extraction distribution ratio(Dc) in acetonitrile-water-alkane extraction system was investigated for IAA-NR-metal chelate. Both kinds of dependence are linear, which suggests that the retention of the electroneutral metal chelates on Novapak $C_{18}$ column is largely due to the hydrophobic effect.

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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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Determination of ${\beta}$-sitosterol in Unsaponifiable Fraction of Zea mays and Related Drug Preparations by HPLC (HPLC에 의한 Zea mays 불검화추출물과 그의 함유제제 중 ${\beta}$-시토스테롤의 정량)

  • Kim, Kyeong-Ho;Park, Woo-Sun;Shim, Chang-Gu
    • YAKHAK HOEJI
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    • v.40 no.2
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    • pp.149-154
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    • 1996
  • A high-performance liquid chromatographic method for the determination of ${\beta}$-sitosterol in the unsaponifiable fraction of Zea mays L. and its related drug preparations using a cholesterol as an internal standard was investigated. They were saponified with 20% methanolic KOH solution. Phytosterols in the reaction mixture were extracted with diethyl ether and separated on silica gel TLC plate with n-hexane-diethyl ether(40:60) as the solvent and then were scraped off. They were separated by reversed phase high perfomance liquid chromatography on Inertsil ODS-2 column with detection at 205nm. Cholesterol and ${\beta}$-sitosterol were resolved from interferences by adjusting the acetonitrile content in the MeOH-tetrahydrofuran-$H_2O$ eluent. The detection limit of ${\beta$-sitosterol was 0.43${\mu}$g.

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Residue of Clindamycin in the Muscles of Eel and Flounder Infected by Streptococcus sp. by HPLC

  • Jang, Won-Cheoul;Shim, Sang-Kyun;Heo, Gang-Joon
    • Toxicological Research
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    • v.13 no.3
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    • pp.209-213
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    • 1997
  • Residue and recoveries of clindamycin were investigated by reversed-phase high performance liquid chromatography (RP-HPLC) which was infected for the control of streptcoccal infection in Anguilla japonica and Paralichthys olivaceusis. Detection limit was 0.1 ppm. Recoveries of clindamycin in muscles of flounder and eel were 80.4 and 78.8%, respectively. The clindamycin in eel and flounder was detected up to 13 and 15 days after dosing, respectively.

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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.

Determination of eugenol in Eugenia caryophyllata by high-performance Liquid chromatography with photodiode array detection and method validation (HPLC-PDA를 이용한 정향(Eugenia caryophyllata) 중의 eugenol 분석법 확립 및 검증)

  • Yun, Hyeong-Jun;Yun, So-Mi;Lee, Myoung-Heon;Son, Seong-Wan
    • Korean Journal of Veterinary Research
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    • v.48 no.1
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    • pp.9-16
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    • 2008
  • A method for the quantification of eugenol in the medicinal herb Clove was developed and validated. For preparation of sample solutions clove was dried at $60^{\circ}C$ for 2h and ground by mixer and extracted with 95% ethanol for shaking extraction. The elutes were analyzed by HPLC system included a reversed phase column, a isocratic mobile phase of 60% methanol and PDA detector set at 280 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $0.0125~1{\mu}g/ml$. The limit of detection per sample injection ($20{\mu}l$) was $0.81ng/{\mu}l$ and limit of quantification was $2.47ng/{\mu}l$. The method showed good intra-day precision (%RSD 0.08 ~ 0.27%) and inter-day precision (%RSD 0.32 ~ 1.19%).

Analysis of Lignans in Acanthopanax sessiliflorus Fruits and Their Fermented Wine by HPLC

  • Kim, Hye-Min;Kim, Ju-Sun;Cho, Seon-Haeng;Kang, Sam-Sik;Cheoi, Dae-Sung;Lee, Sang-Hyun
    • Korean Journal of Medicinal Crop Science
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    • v.14 no.5
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    • pp.289-292
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    • 2006
  • High performance liquid chromatography (HPLC) was used for the determination of lignans, eleutherosides B and E, in Acanthopanax sessiliflorus fruits and their fermented wine. The lignans were quantified by a reversed-phase system using a gradient of $H_2O$ and acetonitrile as a mobile phase within 20 min. The analysis was successfully carried out within 20 min. The contents of eleutherosides Band E as main active principles of Acanthopanax species were measured in A. sessiliflorus fruits (1.15 and $8.49\;{\mu}g/mg$, respectively), their fermented wine (0.45 and $1.33\;{\mu}g/mg$, respectively) and wine residues (no detection).

Reversed-Phase Ion-Pair High Performance Liquid Chromatographic Elution Behavior of Noble Metal-Thiacrown Ether Complexes (귀금속-티아크라운에테르 착물들의 역상 이온쌍 고성능 액체크로마토그래피 용리거동)

  • Chung, Yong Soon;Kim, Dong Won;Lee, Kang Woo;Kim, Chang Seok
    • Journal of the Korean Chemical Society
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    • v.42 no.4
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    • pp.416-421
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    • 1998
  • In the reversed-phase ion-pair high performance liquid chromatographic (RPIP-HPLC) elution behavior of noble metal-thiacrown ether complexes, the effects of the concentration of ion-pairing reagent and kind of ligands were studied. It was found that the less the number of atoms in the ring of the thiacrown ether molecule was, the larger the selectivity was, and the elution mechanism of the complexes was explained due to the formation of ion-pair when the concentration of sodium dodecyl sulfate (SDS) in mobile phase was lower than 10 mM and due to the formation of micelle when the SDS concentration was higher than 10 mM. As a conclusion, separations of the noble metal-thiacrown ether complexes in an optimum separation condition were accomplished successfully and the method was proved to be an useful one for the separation and determination of Ag (Ⅰ) ion in a black-white photographic fixing solution.

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Separation of D and L Amino Acids by High-Performance Liquid Chromatography

  • Lee, Sun-Haing;Ryu, Jae-Wook;Park ,Kyoung-Sug
    • Bulletin of the Korean Chemical Society
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    • v.7 no.1
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    • pp.45-50
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    • 1986
  • Separation of optical isomers of some derivatives of amino acids by reversed-phase HPLC has been accomplished by adding a chelate of an optically active amino acid to copper(Ⅱ) to the mobile phase. Cu(Ⅱ) complexes of L-proline and L-hydroxyproline in the mobile phase showed different degrees of separation. Optical isomers of DNS derivatives of amino acids are selectively separated, but those of several other derivatives are not at all. The kinds of buffer agents, the pH, and the concentrations of acetonitrile and the Cu(Ⅱ) ligand all affect the separations. The elution behavior between D and L DNS-amino acids appears to depend on the alkyl side chain of the amino acids. A chromatographic mechanism is proposed that is based on a stereospecificity of the formation of ternary complexes by the D, L-DNS-amino acids and the chiral additive associated with the stationary phase. The steric effects of the ligand exchange reactions are related with the feasibility of cis and/or trans attack of the amino acids to the binary chiral chelate retained on the stationary phase.

Quantitative Analysis of Platycodin D from Platycodon grandiflorum by HPLC-ELSD (HPLC-ELSD법에 의한 길경의 platycodin D 정량분석)

  • Kim, Geum-Soog;Kim, Hyun-Tae;Seong, Jae-Duck;Park, Hee-Saeng;Kim, Soo-Dong
    • Korean Journal of Medicinal Crop Science
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    • v.10 no.3
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    • pp.200-205
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    • 2002
  • Platycodin D was isolated from n-butanol extract of Platycodi radix(Platycodon grandiflorum and identified by the spectroscopic analysis using $^1H$ and $^{13}C$ NMR techniques. A new method of analysis of platycodin D by high performance liquid chromatography(HPLC) was established using a reversed phase system with YMC-Pack ODS-AM( 250 X 4.6 mm) column and 30% acetonitrile as a mobile phase. Evaporative light scattering detector was used as detector. The kinds of extraction solvents and methods were examined to determine the efficient extraction condition and HPLC analysis was carried out to establish the optimum drying condition for the root of Platycodon grandiflorum. The contents of Platycodin D was highest as 0.083% when platycodon roots were dried at $60^{\circ}C$ using dry oven.