• Title/Summary/Keyword: reversed phase

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Centrifugal Liquid Chromatography with Application of the N-hexadecyl-L-proline Coated Reversed Phase for Separation of amino Acid Enantiomers (N-hexadecay-L-proline이 코팅된 역상 원심 액체크로마토그래피에 의한 아미노산 이성질체의 분리)

  • Sun Haing Lee;Tae Sub Oh;Hae Woon Lee
    • Journal of the Korean Chemical Society
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    • v.36 no.6
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    • pp.849-856
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    • 1992
  • We prepared a simple, economic and versatile preparative system for an enantiomeric separation. Hydrophobic amino acid enantiomers were resolved in the preparative scale by a centrifugal liquid chromatography on the N-hexadecyl-L-proline coated reversed phase. The factors controlling the retention and resolution of racemic amino acids such as the concentration of Cu(Ⅱ), pH of the eluent, the type and content of organic modifier, and rpm of CLC were examined. Several mg of hydrophobic amino acid enantiomers were separated preparatively. To separate all of different amino acid enantiomers, various coating material will be investigated.

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Determination of Rosmarinic Acid and Caffeic Acid from Perilla frutescens var. japonica and var. acuta by Reversed-Phase HPLC (RP-HPLC를 이용한 백소엽(白蘇葉)과 자소엽(紫蘇葉)의 카페익산과 로즈마린산 분석)

  • Kim, Byung-Youn;Jeong, Ji-Seon;Kwon, Ha-Jeong;Lee, Je-Hyun;Hong, Seon-Pyo
    • The Korea Journal of Herbology
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    • v.23 no.3
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    • pp.67-72
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    • 2008
  • Objectives : This study presents a high performance liquid chromatography methods for the quantitative and qualitative analysis of rosmarinic acid (RA) and caffeic acid (CA) in Perilla frutescens var. japonica and var. acuta. Methods : Chromatographic separation was performed using a mixture of methanol, water and formic acid (35 : 64.2 : 0.8) with a reversed-phase column (Gemini C18, 4.6 ${\times}$ 150 mm, 3 ${\mu}m$). The analyses were detected at UV (280 nm). Results : The samples were extracted with 50% EtOH under reflux for 1 h, and simultaneous determination for RA and CA in hyang-so-san and haeng-so-san was possible without interference peaks Conclusions : According the results, we developed a determination method for RA and CA in Perillae Folium. Owing to Perilla frutescens var. japonica and var. acuta did not show significant difference in contents of RA and CA, both Perilla frutescens could be available as herbal medicine.

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Comparison of 2-D RP-RP MS/MS with 1-D RP MS/MS for Proteomic Analysis (단백체 분석을 위한 일차원 및 이차원 역상크로마토그래피의 비교)

  • Moon, Pyong-Gon;Cho, Young-Eun;Baek, Moon-Chang
    • YAKHAK HOEJI
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    • v.54 no.5
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    • pp.377-386
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    • 2010
  • Single-dimensional (1-D) and two-dimensional (2-D) LC methods were utilized to separate peptides from various sources followed by MS/MS analysis. Two-dimensional ultra-high performance liquid chromatography is a useful tool for proteome analysis, providing a greater peak capacity than 1-D LC. The most popular 2-D LC approach used today for proteomic research combines strong cation exchange and reversed-phase LC. We have evaluated an alternative mode for 2-D LC of peptides using 2-D RP-RP nano UPLC Q-TOF Mass Spectrometry, employing reversed-phase columns in both separation dimensions. As control experiments, we identified 129 proteins in 1-D LC and 322 proteins in 2-D LC from E. coli extract peptides. Furthermore, we applied this method to rat primary hepatocyte and a total of 170 proteins were identified from 1-D LC, and 527 proteins were identified from all 2-D LC system. The in-depth protein profiling established by this 2-D LC MS/MS from rat primary hepatocyte could be a very useful reference for future applications in regards to drug induced liver toxicity.

Effects of Microstructure on the Fatigue Crack Propagation Resistance in Dual Phase Steel (複合組織鋼 의 피勞균열進展抵抗 에 미치는 微視組織 의 영향)

  • 김정규;황돈영;박승락
    • Transactions of the Korean Society of Mechanical Engineers
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    • v.8 no.1
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    • pp.34-40
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    • 1984
  • In this study, martensite-ferrite dual phase steel composed of martensite in hard phase and ferrite in soft phase is made as model material, and the difference of fatigue crack propagation behavior resulted from the structural size is investigated by fracture mechanics and microstructural method. The main results obtained are as follows; 1)Fatigue crack propagation rate is influenced by ferrite grain size. In other words, in the low .DELTA. K region fatigue crack propagation rate is decreased with decreasing of grain size but the difference of propagation rate resulted from the structural size is decreased as .DELTA.K is increased. 2)The above result is explained by the degree of crack arrest effect of second phase for fatigue crack propagation depending on the ratio of reversed plastic zone size to ferrite grain size.

Microstructurally sensitive crack closure (微視組織에 敏感한 균열닫힘 현상)

  • 김정규;황돈영
    • Transactions of the Korean Society of Mechanical Engineers
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    • v.10 no.6
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    • pp.898-905
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    • 1986
  • In order to obtain the microstructure improving fatigue crack propagation resistance of steels, fatigue crack propagation behavior of martensite-ferrite dual phase steels is investigated in terms of crack deflection and crack closure. The results obtained are as follows; (1) .DELTA.K$_{th}$ and fatigue crack propagation resistance in low .DELTA.K region increases with increasing hardness of second phase. But the difference of this crack propagation resistance decreases with increasing .DELTA.D. (2) In low .DELTA.K region, crack closure increases with increasing hardness of second phase, when the materials have all the sam volume fractionof second phase, or when yield strengths are similar in all materials. (3) These crack closure can be explained by fracture surface roughness due to crack deflection.n.

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.

Effect of Reverse Transformation on the Damping Capacity of High Manganease Austenitic Stainless Steel (고 Mn 오스테나이트계 스테인리스강의 감쇠능에 미치는 역변태의 영향)

  • Kang, C.Y.
    • Journal of Power System Engineering
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    • v.16 no.4
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    • pp.60-65
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    • 2012
  • This study was carried out to investigate the effect of reverse transformation on the damping capacity in high manganese austenitic stainless steel. ${\alpha}^{\prime}$-martensite was formed with the specific direction and surface relief by deformation. Over 95% of the austenite phase was transformed to deformation-induced ${\alpha}^{\prime}$-martensite by 70% cold rolling. Reverse transformation became rapid above an annealing temperature of $550^{\circ}C$, but there was no significant transformation above $700^{\circ}C$. In addition, with increasing annealing time at $700^{\circ}C$, reverse transformation was induced rapidly, but the transformation was almost completed at 10 min. Damping capacity was increased up to $700^{\circ}C$, and than unchanged with the increasing annealing temperature. Damping capacity increased steeply with an increasing reverse treatment time up to 10min, whereas there were no significant change with a treatment time of more than 10 min. Damping capacity increased with an increasing the reversed austenite and was strongly affected by reversed austenite.

Quantitative Analysis of Lovastatin in Human Plasma and urine by Reversed-Phase High-Performance Liquid Chromatography (역상 고속액체크로마토그라프법을 이용한 혈장 및 뇨 중 로바스타틴의 정량)

  • Choi, Hye-Jin;Kim, Myoung-Min;Choi, Kyung-Eob
    • YAKHAK HOEJI
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    • v.42 no.5
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    • pp.473-479
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    • 1998
  • Lovastatin (LOVA), a fungal metabolite isolated from cultures of Aspergillus terreus, is a competitive HMG-CoA reductase inhibitor used for the treatment of primary hyper cholesterolemia, and has also been shown to suppress growth in a variety of non-glioma tumor cell lines. A sensitive reversed-phase high-perfonnance liquid chromatographic method with ultraviolet (UV) absorbance detection has been developed to quantitate LOVA in human plasma and urine samples using liquid-liquid extraction procedure. Baseline separation of LOVA and internal standard, simvastatin was achieved on a Novapak $C_{18}$ analytical column with a mobile phase containing 0.025M $NaH_2PO_4$: CAN (35:65, v/v%), adjusted pH to 4.5. The flow rate was set at 1.5ml/min, and the column effluent was monitored by a UV detection at 238nm. The limit of quantification was determined to be 0.5${\mu}$g/ml while extraction efficiency of LOVA ranged from 73.4-82.9% at LOVA concentrations of 0.5 to 10${\mu}$g/ml. Good linearity with correlation coefficients greater than 0.999 was obtained in the range of LOVA concentrations from 0.5 to 10${\mu}$g/ml. The accuracy and the precision were proven excellent with relative standard deviation (RSD, %) and relative error (RE, %) of less than 4.2 and 4.0, respectively. Intraday precision, evaluated at five LOVA concentrations (0.5, 1, 2, 5, 10${\mu}$g/ml) and expressed as RSD ranged from 0-1.82% while the interday precision at the same concentrations ranged from 0.7-10.5%. The analytical method described was then successfully employed for the determination of LOVA concentrations in plasma samples obtained during a phase II clinical trial using high doses of LOVA (30-40mg/kg/day). This method could be further utilized for the ongoing pharmacolkinetic studies and therapeutic drug monitoring of the high-dose LOVA therapy in adenocarcinoma patients.

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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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Separation of Two Amino Acids by Microemulsion Bulk Liquid Membrane

  • Salabat, Alireza;Sanij, Fereshteh Dehghani
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3387-3390
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    • 2012
  • In this research work the potentialities of microemulsion bulk liquid membrane for the selective transport of L-tryptophan (L-Trp) and L-tyrosine (L-Tyr) are investigated at 298.15 K. Reversed micelle formed by sodium bis(2-ethylhexyl)sulfosuccinate (AOT) in dichloroethane, was used as mobile carrier to transport amino acids between a source and a receiving aqueous phase. The effects of pH, surfactant concentration and initial amino acid concentration on the extraction efficiency and transfer rate of the amino acids were studied. It is verified that for a mixture of two amino acids, L-Trp can be extracted selectively by using this type of the bulk liquid membrane with optimized condition.