• Title/Summary/Keyword: Chromatographic retention

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Osmotic Cross Second Virial Coefficient ($B_{23}$) of Unfavorable Proteins: Modified Lennard-Jones Potential

  • Choi, Sang-Ha;Bae, Young-Chan
    • Macromolecular Research
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    • v.17 no.10
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    • pp.763-769
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    • 2009
  • A chromatographic method is used to measure interactions between dissimilar proteins in aqueous electrolyte solutions as a function of ionic strength, salt type, and pH. One protein is immobilized on the surface of the stationary phase, and the other is dissolved in electrolyte solution conditions flowing over that surface. The relative retention of proteins reflects the mean interactions between immobile and mobile proteins. The osmotic cross second virial coefficient calculated by assuming a proposed potential function shows that the interactions of unfavorable proteins depend on solution conditions, and the proposed model shows good agreement with the experimental data of the given systems.

Molecularly Imprinted Monolithic Stationary Phases for Liquid Chromatographic Separation of Tryptophan and N-CBZ-Phenylalanine Enantiomers

  • Yan, Hong-Yuan;Row, Kyung-Ho
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.11 no.4
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    • pp.357-363
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    • 2006
  • Monolithic molecularly imprinted columns were designed and prepared by an in-situ thermal-initiated copolymerization technique for rapid separation of tryptophan and N- CBZ-phenylalanine enantiomers. The influence of polymerization conditions and separation conditions on the specific molecular recognition ability for enantiomers and diastereomers was investigated. The specious molecular recognition was found to be dependent on the stereo structures and the arrangement of functional groups of the imprinted molecule and the cavities in the molecularly imprinted polymer (MIP). Moreover, hydrogen bonding interactions and hydrophobic interactions played an important role in the retention and separation. Compared to conventional MIP preparation procedures, the present method is very simple, and its macroporous structure has excellent separation properties.

Membrane for the Removal of Volatile Organic Compounds from Air (대기중의 휘발성 유기물 제거용 분리막)

  • Deng, S.;Lang, K.;Wang, J.;Tremblay, A.;Matsuura, T.
    • Membrane Journal
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    • v.7 no.1
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    • pp.22-30
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    • 1997
  • Porous asymmetric membranes were prepared from polyetherimide polymer by the phase-inversion technique under different conditions. The performance of the membranes was tested for the removal of acetone vapour from nitrogen. A membrane which showed a high acetone permeability and a high selectivity was chosen and tested further for the separation of different organic vapours from nitrogen. The molecular structure of organic vapours and the selectivity were correlated. A strong correlation was also found between the chromatographic retention time of the organic vapour and the selectivity. These experimental results led to the conclusion that the sorption is the factor governing the separation of volatile organic compounds from nitrogen. A membrane was also prepared by coating the surface of a porous polyetherimide membrane with silicone rubber. The performance of membranes with and without silicone rubber coating was compared.

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High Performance Liquid Chromatographic Analyses of Higenamine Enantiomers in Aconite Roots

  • Chung, Kyo-Soon;YunChoi, Hye-Sook;Hahn, Young-Hee
    • Natural Product Sciences
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    • v.6 no.1
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    • pp.20-24
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    • 2000
  • The enantiomers of higenamine were directly separated by high performance liquid chromatography using a chiral stationary phase and detected by UV. The R- and S-isomers of higenamine were eluted at the retention time of 22 min and 27 min, respectively. Higenamine was determined to be present as R-(+)-enantiomer not only in the embryo of Nelumbo nucifera, from which the separation of R-(+)-higenamine was reported, but also in various Aconite roots, from which higenamine was separated as optically inert racemic mixtures.

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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
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    • v.29 no.6
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    • pp.375-379
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    • 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.

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Quantitative Determination of Salidroside and Tyrosol from the Underground Part of Rhodiola rosea by High Performance Liquid Chromatography

  • Linh, Pham-Tuan;Kim, Young-Ho;Hong, Seon-Pyo;Jian, Jiang-Ji;Kang, Jong-Seong
    • Archives of Pharmacal Research
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    • v.23 no.4
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    • pp.349-352
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    • 2000
  • A reversed-phase high performance liquid chromatographic method was developed to determine salidroside and tyrosol simultaneously in the Rhodiola rosea. The optimum condition was Nova-pak $C_18$as stationary phase, 6.5% methanol in water as mobile phase and detection at UV 225 nm. The identification was carried out by comparing the retention time and LC/MS spectrum of the relevant peaks with those of isolated standards. The contents of salidroside and tyrosol in the samples gathered from various area in China were ranged over 1.3-11.1 ${m}g/g$ and 0.3-2.2 ${m}g/g$, respectively.

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Problem-solving approach for salbutamol analysis by HPLC during pharmaceutical assay

  • Gholizadeh-Hashjin, Aiesheh;Hamishehkar, Hamed;Monajjemzadeh, Farnaz
    • Analytical Science and Technology
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    • v.35 no.5
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    • pp.189-196
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    • 2022
  • When cationic basic compounds are chromatographed using hydro-organic mobile phase, the presence of anionic free silanols in the silica-based stationary phases results in broad and asymmetrical peaks. The addition of an ionic reagent to the mobile phase prevents analytes from accessing free silanols, improving peak shape. In this study, the chromatographic behavior of salbutamol sulfate as a basic compound was investigated under various conditions, including the use of different columns, mobile phases, and ion-pair reagents such as triethanolamine (TEA) and sodium heptane sulfonate (SHS). The retention and peak shape of chromatograms were both evaluated. The results show that pre-conditioning the column with TEA and including it in the mobile phase can prevent cationic analytes from accessing anionic silanols, resulting in improved peak shape. Furthermore, buffering the mobile phase is an important factor in keeping the pH constant throughout the process. The chosen method was validated in part. This study could be helpful for researchers and analyst to solve such problems with cationic basic components.

Chromatographic Separation of Hydrogen Isotopes by Deactivated Alumina Stationary Phase (비활성 알루미나 고정상을 이용한 수소동위원소의 크로마토그래피 분리)

  • Kim, Kwang Rag;Lee, Sung Ho;Kang, Hee Suk;Chung, Hongsuk;Sung, Ki Woung
    • Applied Chemistry for Engineering
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    • v.9 no.1
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    • pp.121-128
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    • 1998
  • In fields of operating or handling a hydrogen isotope facility, and of the technology for nuclear fusion source management, gas chromatography has been used as one of the practical techniques lot separation and enrichment of hydrogen isotopic gases including tritium. Chromatographic separation experiments of the hydrogen isotope mixture (hydrogen, deuterium and tritium) were carried out by use of a commercially available gas chromatograph. An aliquot of gas sample was injected by a specially designed vacuum sampler into the stream of inert carrier gas which went through the separation column under liquid nitrogen temperature. The complete separation of hydrogen isotopic molecules was observed with an alumina adsorbent partially deactivated by coating with 10% manganese chlorine. In addition, fairly good separation conditions were obtained without any appearance of nuclear spin isomers with shorter retention time, which would be available for the practical applications of the hydrogen isotope separation and enrichment.

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Preparation of Cucurbituril Anchored Silica Gel by Cross Polymerization and Its Chromatographic Applications

  • Cheong, Won-Jo;Go, Joung-Ho;Baik, Yoon-Suk;Kim, Sung-Soon;Nagarajan, Erumaipatty R;Selvapalam, Narayanan;Ko, Young-Ho;Kim, Ki-Moon
    • Bulletin of the Korean Chemical Society
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    • v.29 no.10
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    • pp.1941-1945
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    • 2008
  • A new chromatographic stationary phase has been prepared by cross polymerization between allylsilica and perallyloxycucurbit[6]uril and characterized by elemental analysis and FT-IR spectroscopy. The double endcapping has been proven to improve the separation efficiency of the cucurbituril-based stationary phase material. The first end-capping was carried out when allylsilica was made. The second end-capping was done as the final step of the whole process, and the use of a mixture of hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) as an end-capping reagent was found better than the use of only HMDS or TMCS. Our stationary phase has shown generally good results in separation of nonpolar and polar analytes. This phase showed even better separation performance than the commercial C18 phase for the case where hostguest chemistry was properly incorporated in solute retention.

High Performance Liquid Chromatographic Assay of a New Fluoroquinolone, LB20304, in the Plasma of Rats and Dogs

  • Seo, Mi-Kyeong;Jeong, Yi-Na;Kim, Hoon-Joo;Kim, In-Chull;Lee, Yong-Hee
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.554-558
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    • 1996
  • High-performance liquid chromatographic method was developed for the determination or LB 20304 (compound 1) in the plasma of rats and dogs. The analyte was deproteinized with 1 volume of methanol and 1/2 volume of 10% zinc sulfate, and the supernatant was injected onto a reversed-phase HPLC column. The mobile phase was a mixture of 24 parts of acetonitrile and 76 parts of 0.1% trifluoroacetic acid. The flow rate was 1 ml/min, and the effluent was monitored by fluorescence detector at an excitation wavelength of 337 nm and an emission wavelength of 460 nm. The retention time of compound 1 was 6.3 min. The assay of compound 1 was linear over the concentration range of 0.2-100.mu.g/ml in the plasma of rats and dogs. The lower limit of quantification was 0.2.mu.g/ml using 100.mu.l of plasma with a 97-99% accuracy and a 12-14% precision. In the 0.5, 5, and 50.mu.g/ml quality control samples, the intra- and inter-day accuracy were 88-95% and 88-97%, whereas intra- and interday precision were 0.5-6.6% and 0.2-9.3%, respectively, in the plasma of rats and dogs. The recoveries were 68-71% independent of concentration and species in the plasma. No interferences from endogenous substances were observed. Taken together, the above HPLC assay method by deproteinization and fluorescence detection was suitable for the determination of compound 1 in the preclinical pharmacokinetics.

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