• 제목/요약/키워드: Stationary phase

검색결과 773건 처리시간 0.02초

고속역류크로마토그래피 기술을 이용한 생리활성 물질의 분리 및 정제 (Isolation and Purification of Bioactive Materials Using High-Performance Counter-Current Chromatography (HPCCC))

  • 정동수;신현재
    • KSBB Journal
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    • 제25권3호
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    • pp.205-214
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    • 2010
  • 역류크로마토그래피 (counter-current chromatography, CCC)는 일련의 분배과정을 한 개의 튜브 내에서 연속적으로 일어나도록 고안된 시스템으로서 컬럼으로는 polytetrafluoroethylene(PTFE) 튜브가 다층으로 감겨있는 원통형의 홀더 3개가 서로 기어를 통해 물려있으며, 홀더가 회전과 공전을 통해 튜브의 꼬임을 방지하는 rotary seal-free flow centrifuge 시스템으로 되어있다. 역상 HPLC (reverse phase HPLC)에서는 고정상이 실리카에 결합된 유기물단 (organic moiety)이 수용성 이동상 물질에 의해서 용매화 (solvated)되는 반면 CCC는 실리카 대신에 강한 중력장에 의해 분리되는 자유로운 용매가 고정상이 되며 이 고정상의 부피비율은 20-30%에 이른다. 즉 고체담체에 결합된 유기관능기 대신에 물과 섞이지 않는 hexane 같은 유기용제가 고정상으로 사용되는 것이다. 고속역류크로마토그래피 (high-performance countercurrent chromatography, HPCCC)는 CCC의 기능을 향상시킨 분리시스템으로서 높은 중력장하에서 높은 이동상 속도와 높은 분리효율과 짧은 분리시간을 특징으로 하고 있다. 특히 mg 단위에서 kg 단위로의 스케일업이 선형적으로 가능하다는 큰 장점을 지니고 있다. 이 총설에서는 현재까지 개발된 CCC의 일반적인 이론을 간략히 정리하고 최신 HPCCC 장비의 적용 예를 살펴보고 그 응용분야로서 생리활성물질의 분리 및 정제와 관련된 연구동향을 정리하였다.

HILIC 분석법 개발을 위한 지능형 솔루션 (Hydrophilic Interaction Liquid Chromatography)

  • Matt James;Colin Pipe;Mark Fever;Jen Field;Seungho Chae
    • FOCUS: LIFE SCIENCE
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    • 제1호
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    • pp.6.1-6.9
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    • 2024
  • The document is a white paper on Hydrophilic Interaction Liquid Chromatography (HILIC) analysis method development. HILIC is a type of chromatography that uses an organic/aqueous mobile phase and a polar stationary phase. In HILIC, water is a strong solvent, and unlike in Reversed Phase Liquid Chromatography (RPLC), increasing the proportion of water in the mobile phase reduces the retention time of the analyte. The paper discusses when to consider HILIC analysis methods, the advantages of HILIC, and the challenges often encountered due to the lack of understanding of HILIC mechanisms compared to RPLC. It also provides a systematic flowchart for intelligent solutions for HILIC analysis method development, which includes a three-step approach for chromatography analysis method development. The first step involves gathering as much information as possible about the analyte (e.g., pKa, log P, log D). The second step involves analyzing the sample under different pH conditions using three HILIC columns in either isocratic or gradient mode to identify the suitable column/pH combination for the analyte. The third step involves optimizing the separation by investigating other parameters such as temperature and ionic strength, and assessing the robustness of the method. The paper emphasizes that the selection of the appropriate stationary/mobile phase combination, based on the differences between the HILIC stationary phases and the mobile phase pH, can provide high selectivity in the analysis. This step-by-step approach can help users develop an efficient analysis method.

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Separation of the Enantiomers of β-Blockers Using Brush Type Chiral Stationary Phase Derived from Conformationally Rigid α-Amino β-Lactam

  • Pirkle, William H.;Lee, Won-Jae
    • Bulletin of the Korean Chemical Society
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    • 제31권3호
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    • pp.620-623
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    • 2010
  • A brush type chiral stationary phase (CSP 2) derived from ${\alpha}$-amino ${\beta}$-lactam was prepared for the separation of the enantiomers of ${\beta}$-blockers. Compared to the CSP derived from ${\alpha}$-amino phosphonate (CSP 1), in general, the conformationally rigid CSP 2 showed greater scope and much enhanced enantioselectivity for the resolution of ${\beta}$-blockers. The effect of various salt additives on enantioseparation of ${\beta}$-blockers in the mobile phase was investigated. The unusual effect of temperature on the chromatographic behaviors was observed on CSP 2. It also afforded appreciable increases in enantioselectivity without significantly affecting resolution, as the column temperature was reduced.

An Improved Stationary Frame-based Digital Current Control Scheme for a PM Synchronous Motor

  • Kim Kyeong-Hwa;Youn Myung-Joong
    • 전력전자학회:학술대회논문집
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    • 전력전자학회 2001년도 Proceedings ICPE 01 2001 International Conference on Power Electronics
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    • pp.174-178
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    • 2001
  • An improved stationary frame-based digital current control technique for a permanent magnet (PM) synchronous motor is presented. Generally, the stationary frame current controller is known to provide the advantage of a simple implementation. However, there are some unavoidable limitations such as a steady-state error and a phase delay in the steady-state. On the other hand, in the synchronous frame current regulator, the regulated currents are dc quantities and a zero steady-state error can be obtained through the integral control. However, the need to transform the signals between the stationary and synchronous frames makes the implementation of a synchronous frame regulator complex. Although the PI controller in the stationary frame gives a steady-state error and a phase delay, the control performance can be greatly improved by employing the exact decoupling control inputs for the back EMF, resulting in an ideal steady-state control characteristics irrespective of an operating condition as in the synchronous PI decoupling controller. However, its steady-state response may be degraded due to the inexact cancellation inputs under the parameter variations. To improve the control performance in the stationary frame, the disturbance is estimated using the time delay control. The proposed scheme is implemented on a PM synchronous motor using DSP TMS320C31 and the effectiveness is verified through the comparative simulations and experiments.

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An Improved Stationary Frame-based Digital Current Control Scheme for a PM Synchronous Motor

  • Kim, Kyeong-Hwa;Young, Myung-Joong
    • Journal of Power Electronics
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    • 제1권2호
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    • pp.88-98
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    • 2001
  • An improved stationary frame-based digital current control technique for a permanent magnet(PM) synchronous motor is presented. Generally, the stationary frame current controller is known to provide the advantage of a simple implementation. However, there are some unavoidable limitations such as a steady-state error and a phase delay in the steady-state. On the other hand, in the synchronous frame current regulator the regulated currents are dc quantities and a zero steady-state error can be obtained through the integral control. However, the need to transform the signals between the stationary and synchronous frames makes the implementation of a synchronous frame regulator complex. Although the PI controller in the stationary frame gives a steady-state error and a phase delay, the control performance can be greatly improved by employing the exact decoupling control inputs for the back EMF., resulting in an ideal steady-state control characteristics irrespective of an operating condition as in the synchronous PI decoupling controller. However, its steady-state response may be degraded due to the inexact cancellation inputs under the parameter variations. To improve the control performance in the stationary frame, the disturbance is estimated using the time delay control. The proposed scheme is implemented on a PM synchronous motor using DSP TMS320C31 and the effectiveness is verified through the comparative simulations and experiments.

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아미노산 광학이성질체 분리를 위한 가스크로마토그라피용 키랄 고정상의 개발 -새로운 diamide계 키랄 고정상의 응용- (Development of Chiral Stationary Phases for the Gas Chromatographic Separation of Amino Acid Enantiomers New diamide chiral stationary phase)

  • 박만기;양정선;이미영
    • 약학회지
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    • 제33권2호
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    • pp.129-139
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    • 1989
  • New diamide chiral stationary phases of four systematically substituted optically active N-(N-benzoyl-L-amino acid)-anilide synthesized from L-valine, L-leucine, L-isoleucine, and L-phenylalanine were described. The behaviors of these diamides as optically active stationary phases for the separation of N-trifluoroacetyl-D,L-amino acids were examined with respect to separation factors(${\alpha}$) and thermodynamic properties of interaction. The separation of twelve N-trifluoroacetyl-D,L-amino acid isopropyl esters were improved by the order of N-(N-benzoyl-L-leucyl)-anilide>N-(N-benzoyl-L-isoleucyl)-anilide>N-(N-benzoyl-L-valyl)-anilide>N-(N-benzoyl-L-phenylalanyl)-anilide. Eight amino acid derivatives with non-polar R-group and threonine, serine, aspartic acid, and glutamic acid enantiomers were separated on N-(N-benzoyl-L-leucyl)-anilide as chiral stationary phase with good separation factor between 1.07-1.25. The separation factors decreased with respect to increasing column temperature. Possible working temperature of diamide phase was between $130-190^{\circ}C$ for N-(N-benzoyl-L-phenylalanyl)-anilide and $130-180^{\circ}C$ for other three diamide phases. The differential Gibb's free energy (${\Delta}{\Delta}G$) of enantiomers was in the range of -100--180 cal/mol for ten amino acids and -40--60 cal/mol for alanine and aspartic acid.

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Antagonistic Potential of Native Trichoderma viride Strain against Potent Tea Fungal Pathogens in North East India

  • Naglot, A.;Goswami, S.;Rahman, I.;Shrimali, D.D.;Yadav, Kamlesh K.;Gupta, Vikas K.;Rabha, Aprana Jyoti;Gogoi, H.K.;Veer, Vijay
    • The Plant Pathology Journal
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    • 제31권3호
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    • pp.278-289
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    • 2015
  • Indigenous strains of Trichoderma species isolated from rhizosphere soils of Tea gardens of Assam, north eastern state of India were assessed for in vitro antagonism against two important tea fungal pathogens namely Pestalotia theae and Fusarium solani. A potent antagonist against both tea pathogenic fungi, designated as SDRLIN1, was selected and identified as Trichoderma viride. The strain also showed substantial antifungal activity against five standard phytopathogenic fungi. Culture filtrate collected from stationary growth phase of the antagonist demonstrated a significantly higher degree of inhibitory activity against all the test fungi, demonstrating the presence of an optimal blend of extracellular antifungal metabolites. Moreover, quantitative enzyme assay of exponential and stationary culture filtrates revealed that the activity of cellulase, ${\beta}$-1,3-glucanase, pectinase, and amylase was highest in the exponential phase, whereas the activity of proteases and chitinase was noted highest in the stationary phase. Morphological changes such as hyphal swelling and distortion were also observed in the fungal pathogen grown on potato dextrose agar containing stationary phase culture filtrate. Moreover, the antifungal activity of the filtrate was significantly reduced but not entirely after heat or proteinase K treatment, demonstrating substantial role of certain unknown thermostable antifungal compound(s) in the inhibitory activity.

Probing Gamma-ray Emission of Geminga and Vela with Non-stationary Models

  • Chai, Yating;Cheng, Kwong-Sang;Takata, Jumpei
    • Journal of Astronomy and Space Sciences
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    • 제33권2호
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    • pp.75-92
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    • 2016
  • It is generally believed that the high energy emissions from isolated pulsars are emitted from relativistic electrons/positrons accelerated in outer magnetospheric accelerators (outergaps) via a curvature radiation mechanism, which has a simple exponential cut-off spectrum. However, many gamma-ray pulsars detected by the Fermi LAT (Large Area Telescope) cannot be fitted by simple exponential cut-off spectrum, and instead a sub-exponential is more appropriate. It is proposed that the realistic outergaps are non-stationary, and that the observed spectrum is a superposition of different stationary states that are controlled by the currents injected from the inner and outer boundaries. The Vela and Geminga pulsars have the largest fluxes among all targets observed, which allows us to carry out very detailed phase-resolved spectral analysis. We have divided the Vela and Geminga pulsars into 19 (the off pulse of Vela was not included) and 33 phase bins, respectively. We find that most phase resolved spectra still cannot be fitted by a simple exponential spectrum: in fact, a sub-exponential spectrum is necessary. We conclude that non-stationary states exist even down to the very fine phase bins.

Chromatographic Behavior of Proteins on Stationary Phase with Aminocarboxy Ligand

  • Li, Rong;Ju, Ming-Yang;Chen, Bin;Sun, Qing-Yuan;Chen, Guo-Liang;Shi, Mei;Wang, Xiao-Gang;Zheng, Jian-Bin
    • Bulletin of the Korean Chemical Society
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    • 제32권2호
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    • pp.590-594
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    • 2011
  • An aminocarboxy aspartic acid-bonded silica (Asp-Silica) stationary phase was synthesized using L-aspartic acid as ligand and silica gel as matrix. The standard protein mixtures were separated with prepared chromatographic column. The effects of solution pH, salt concentration and metal ion on the retention of proteins were examined, and also compared with traditional iminodiacetic acid-bonded silica (IDA-Silica) column. The results show that Asp-Silica column exhibited an excellent separation performance for proteins. The retention of proteins on Asp-Silica stationary phase was consistent with electrostatic characteristic of cation-exchange. The stationary phase displayed typical metal chelate property after fixing copper ion (II) on Asp-Silica. Under competitive eluting condition, protein mixtures were effectively isolated. Asp ligand showed better ion-exchange and metal chelating properties as compared with IDA ligand.

고성능 액체크로마토그래피의 다당유도체를 기초로 한 키랄 고정상에서 이동상 첨가제가 키랄 아민의 광학분리에 미치는 영향 (Effect of Mobile Phase Additive on Enantiomer Resolution for Chiral Amines on Polysaccharide-derived Chiral Stationary Phases by High Performance Liquid Chromatography)

  • 백만정;윤혜란;이원재
    • KSBB Journal
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    • 제29권3호
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    • pp.205-209
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    • 2014
  • Chromatographic enantiomer resolution of chiral amines was performed on several covalently immobilized and coated chiral stationary phases (CSPs) based on polysaccharide derivatives under the mobile phase conditions containing base or acid or acid/base additive. The chromatographic parameters including separation factors and capacity factors were greatly influenced by the nature of the mobile phase containing base or acid or salt additive as well as the used CSPs. When 0.05% triethylamine/0.05% trifluoroacetic acid as an additive in the mobile phase was used on all CSPs in this study, the greatest enantiomer resolution was observed except for Chiralpak AD. Also, it was shown that the change of base additive into acid or salt in the mobile phase may directly affect chiral recognition mechanisms between the chiral selectors and analytes occurring during enantiomer separation, resulting in the change of elution orders.