• Title/Summary/Keyword: Chromatographic Separation

Search Result 413, Processing Time 0.022 seconds

Chromatographic Separation of Lithum Isotopes by Hydrous Managanese(Ⅳ) Oxide (가수된 산화 망간(Ⅳ)에 의한 리튬 동위원소의 크로마토그래피적 분리)

  • Kim, Dong Won
    • Journal of the Korean Chemical Society
    • /
    • v.45 no.3
    • /
    • pp.219-222
    • /
    • 2001
  • Separation of lithium isotopes was investigated by chemical ion exchange with a hydrous manganese(IV) oxide ion exchanger using an elution chromatography. The capacity of manganese(IV) oxide ion exchanger was 0.5 meq/g. The heavier lithium isotope was enriched in the solution phase, while the lighter isotope was enriched in the ion exchanger phase. The separation factor was determined according to the method of Glueckauf from the elution curve and isotopic assays. The separation factor of $^6Li^+$-$^7Li^+$ isotope pair fractionation was 1.018.

  • PDF

Separation of Amino Acid Enantiomers by Gas Chromatography I With Optically Active N-Benzoyl-L-Valine Derivative as Stationary Phase (가스크로마토그라피에 의한 아미노산 광학이성체의 분리 I 광학활성 N-Benzoyl-L-Valine 유도체의 고정상으로의 응용)

  • 박만기;류재하;강종성
    • YAKHAK HOEJI
    • /
    • v.29 no.6
    • /
    • pp.375-379
    • /
    • 1985
  • The gas chromatographic behavior of optically active N-(N-benzoyl-L-valyl)-anilide used as stationary phase is described. N-(N-benzoyl-L-valyl)-anilide has been synthesized with good yield under mild condition via Schotten-Bauman process and coated on the Chromosorb W AW (80-100mesh) for the purpose of enantiomer separation. The behavior of this compound as optically active stationary phase for the separation of the enantiomers of N-TFA-D, L-amino acid isopropyl esters has been examined with respect to the correlation between the separation factors and column temperatures. All amino acid enantiomers examined were eluted within one hour and the elution pattern showed retention times increasing in the order of alanine, valine, leucine, threonine, proline and methionine.

  • PDF

Chiral Purity Test of Metoprolol Enantiomer After Derivatization with (-)-Menthyl Chloroformate by Reversed-Phase High Performance Liquid Chromatography

  • Kim, Kyeong-Ho;Choi, Pok-Wha;Hong, Seon-Pyo;Kim, Hyun-Ju
    • Archives of Pharmacal Research
    • /
    • v.22 no.6
    • /
    • pp.614-618
    • /
    • 1999
  • A reversed-phase high-performace liquid chromatographic method was developed to determine the optical purity of metoprolol enantiomers. The enantiomers were converted to diastereomeric derivatives using (-)-menthyl chloroformate reagent. Separation of the enantiomers as diastereomers was achieved by reversed-phase HPLC within 30 min using Inertsil C8 column. This method allowed determination of 0.05% of either enantiomer in the presence of its stereoisomer and method validation showed adequate linearity over the required range. Owing to the reaction condition during the derivatization with (-)-menthyl chloroformate, the possibility of racemization had to be established. Different ratios of (S)-(-)-metoprolol and (R)-(+)-metoprolol were prepared. Enantiomeric separation of these mixtures took place on a chiralcel OD column or, after derivatization with (-)-menthyl chloroformate, on a C8 column. The results form the these two independent separation systems were compared with trace racemization and were in very good agreement. No racemization was found during the experiment.

  • PDF

Enrichment of Magnesium Isotopes by Monoazacrown Bonded Merrifield Peptide Resin.

  • Kim, Dong Won
    • Bulletin of the Korean Chemical Society
    • /
    • v.22 no.6
    • /
    • pp.570-574
    • /
    • 2001
  • Magnesium isotope separation was investigated by chemical ion exchange with the 1-aza-12-crown-4 bonded Merrifield peptide resin using an elution chromatographic technique. The capacity of the novel azacrown ion exchanger was 1.0 meq/g dry resin. The heavier isotopes of magnesium were enriched in the resin phase, while the lighter isotopes were enriched in the solution phase. The single stage separation factor was determined according to the method of Glueckauf from the elution curve and isotopic assys. The separation factors of $^{24}Mg^{2+}$-$^{25}Mg^{2+}$, $^{24}Mg^{2+}$-$^{26}Mg^{2+}$, and $^{25}Mg^{2+}$-$^{26}Mg^{2+}$ were 1.008, 1.019, and 1.006, respectively.

Resolution of Aryl α-Aminoalkyl Ketones on a Doubly Tethered Liquid Chromatographic Chiral Stationary Phase Based on (+)-(18-Crown-6)-2,3,11,12-tetracarboxylic Acid

  • Jin, Kab-Bong;Kim, Hee-Jin;Hyun, Myung-Ho
    • Journal of the Korean Chemical Society
    • /
    • v.55 no.5
    • /
    • pp.751-755
    • /
    • 2011
  • A doubly tethered chiral stationary phase (CSP) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid was applied to the resolution of various aryl ${\alpha}$-aminoalkyl ketones with the use of 80% ethanol in water containing 10 mM sulfuric acid as a mobile phase. The chiral resolution was quite successful, the separation factors (${\alpha}$) and the resolutions ($R_S$) being in the range of 1.39-2.05 and 3.18-5.22, respectively. The separation factors (${\alpha}$) on the doubly tethered CSP were slightly worse than those on the corresponding singly tethered CSP. However, the resolutions ($R_S$) on the doubly tethered CSP were generally greater than those on the corresponding singly tethered CSP. The chromatographic behaviors for the resolution of aryl ${\alpha}$-aminoalkyl ketones on the doubly tethered CSP were demonstrated to be dependent on the type and the content of the organic and acidic modifiers in aqueous mobile phase and the column temperature.

Enantioseparation by Sonochromatography

  • Ryoo, Jae-Jeong;Song, Young-Ae;Jeong, Young Han;Hyun, Myung-Ho;Park, Jung-Hag;Lee, Won-jae
    • Bulletin of the Korean Chemical Society
    • /
    • v.27 no.5
    • /
    • pp.637-641
    • /
    • 2006
  • Although chiral separation has been one of the main topics of chromatographic practice for over twenty-five years, it still presents many difficulties. In this work, the ultrasonic dependence of chiral resolution was investigated at various temperatures to improve resolution and reduce analysis time. The chiral resolution was performed on recently commercialized two HPLC chiral stationary phases (CSP 1 and CSP 2) with the analogues of racemic N-acylnaphthylethylamines (1a-d) and racemic amino acid derivatives (2a-c, 3a-c) as analytes. The CSP 1 was prepared from a (R)-N-(3,5-dinitrobenzoyl)phenylglycinol and the CSP 2 was prepared from a (S)-N-3,5-(dinitrobenzoyl) leucine. From the comparison of the chromatographic results under sonic condition with those under non-sonic condition, we found that the ultrasound decreased the elution time in chiral chromatography at all temperatures and improved the enantioselectivity at high temperature (45, 50, 60 ${^{\circ}C}$).

A NUMERICAL STUDY ON THE FLOW CHARACTERISTICS OF GAS CHROMATOGRAPHIC COLUMN (가스 크로마토그래픽 컬럼의 유동특성에 대한 수치적 연구)

  • Kim T.-A.;Kim Youn J.
    • 한국전산유체공학회:학술대회논문집
    • /
    • 2005.10a
    • /
    • pp.21-26
    • /
    • 2005
  • Gas Chromatography (GC) is a wisely technique used for the separation and analysis of liquid and gas sample. Separation of the sample vapors is achieved via their differential migration through a capillary column with an insert carrier gas. The identity and quantity of each vapor in the mixer can be determined from its retention time in the column and a particular property of the gas, such as thermal conductivity, which can be related to the concentration of sample vapor in the carrier gas. Therefore, the flow characteristics in the spiral gas chromatographic column are numerically investigated in this study. Especially, different pressure drop between the front and the rear of GC column with various flow rates is estimated the governing equations are derived from making using of three-dimensional Naver-Stokes equation with incompressible and laminar model due to the nature of low Reynolds number flow. Using a commercial code, FLUENT, the pressure and flow fields in GC column are calculated with various flow rates. The characteristics of thermal cycling which is one of the most important factors affecting the column efficiency and analysis time is also estimated. Furthermore, numerical analyses are also carried out by using commercial code, ANSYS, with various values of power, which is applied to the heating element located at lower GC column.

  • PDF

Sperm Component Inducing 2nd Polar Body Extrusion in Mouse Oocytes (생쥐 난자의 제2극체 방출을 유발하는 정자 성분)

  • 김은희;오현주;손채은;이은주;김동신;여영근;박영식
    • Journal of Embryo Transfer
    • /
    • v.15 no.3
    • /
    • pp.237-245
    • /
    • 2000
  • This study was carried out to elucidate whether sperm contain a factor inducing second polar body extrusion and to search for an effective collection method of the sperm factor Thus, sperm extract, dialyzed sperm-extract or liquid chromatographic fractions of sperm extract was microinjected into ovulated oocytes. And the microinjected oocytes were incubated for 24 hours to investigate about the extrusion of second polar body. The results obtained were as follows; 1. Sperm extract significantly increased the second polar body extrusion. 2. Sperm extract showed five major fractions at retention volumes (RVs) 1.25, 1.37, 1.84, 2.10 and 2.67ml after separation with Superose 12 column. These sperm extract fractions did not significantly increase the second polar body extrusion. 3. Dialyzed sperm-extract significantly increased the second polar body extrusion 4. Dialyzed sperm-extract showed three maior fractions at RVs 1.88, 2.14 and 2.77ml after separation with Superose 12 column. Of these fractions, the fraction RV2.14 significantly increased the second polar body extrusion. In conclusion, sperm extract contained a factor inducing the second polar body extrusion and the factor was contained largely in fraction RV2.14 after dialysis and liquid chromatographic fractionation of sperm extract.

  • PDF

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

  • Paik, Man-Jeong;Yoon, Hye-Ran;Lee, Wonjae
    • KSBB Journal
    • /
    • v.29 no.3
    • /
    • pp.205-209
    • /
    • 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.

Chromatographic Separation of Xanthine Derivatives on Single and Mixed-Template Imprinted Polymers

  • Wang, Dexian;Hong, Seung-Pyo;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
    • /
    • v.25 no.3
    • /
    • pp.357-360
    • /
    • 2004
  • We developed in the present study molecular imprinted polymers (MIPs), using single templates (pentoxifylline, caffeine and theophylline) and mixed-templates (pentoxifylline-caffeine, pentoxifylline-theophylline and caffeine-theophylline). The MIPs were prepared with methacrylic acid (MAA) as the monomer, ethylene glycol dimetharylate (EGDMA) as the crosslinker and 2,2'-azobis(isobutyronitrile) (AIBN) as the initiator. The obtained polymer particles (particle size after grinding was about 25-35 ${\mu}$m) were packed into a HPLC column (3.9 mm i.d. ${\times}$ 150 mm). The selectivity and chromatographic characteristics of the MIPs were studied using acetonitrile as the mobile phase at a flow rate of 0.8 mL/min. UV detector wavelength was set at 270 nm. Different single template MIPs showed different molecular recognitions to the templates and the structurally analogues, according to the rigidity and steric hindrance of the compounds. Recognition was improved on the mixed-template MIPs as a result of the cooperation or sum effect of the templates, whereas on the pentoxifylline-theophylline imprinted polymer, the highest selectivity and affinity were obtained. Separations of the test compounds on different polymers were also investigated.