• Title/Summary/Keyword: mixed stationary phases

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Titanized or Zirconized Porous Silica Modified with a Cellulose Derivative as New Chiral Stationary Phases

  • Seo, You-Jin;Kang, Gyoung-Won;Park, Seong-Tae;Moon, Myeong-Hee;Park, Jung-Hag;Cheong, Won-Jo
    • Bulletin of the Korean Chemical Society
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    • v.28 no.6
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    • pp.999-1004
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    • 2007
  • Spherical porous silica supports modified with titanium or zirconium alkoxides were prepared, and allyl groups were chemically attached to the titanized or zirconized silica supports, and the product was cross-polymerized with a double bond containing cellulose derivative to yield new CSPs (chiral stationary phases). Magic angle spinning 13C solid state NMR and elemental analysis were used to characterize the CSPs. The performances of the chiral stationary phases were examined in comparison with a conventional chiral stationary phase. Spherical porous silica particles modified with 3,5-dimethylphenylcarbamate of cellulose were prepared and used as the conventional chiral stationary phase. Chromatographic data were collected for a few pairs of enantionmers in heptane/2-propanol mixed solvents of various compositions with the three chiral columns and the results were comparatively studied. The separation performance of the chrial phase made of the titanized silica was better than the others, and the separation performance of the chiral phase of the zirconized silica was comparable to that of the conventional chiral phase. The superiority of titanized silica over bare or zirconized silica in chiral separation seemed to be owing to the better yield of crosslinking (monitored by increase of carbon load) for titanized silica than for the others.

Determination of Protein Amino Acids as the N-TFA N-Butyl Esters by Gas Liquid Chromatography (Gas Liquid Chromatography에 의한 단백질 아미노산의 분석)

  • Woo, Kang-Lyung
    • Korean Journal of Food Science and Technology
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    • v.22 no.1
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    • pp.88-93
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    • 1990
  • For effective separation of the N-TFA n-butyl ester amino acids on the stainless steel column by GLC, dual column of the mixed stationary phases, 3.36% OV-17+3.0% SE-30(column 1) and 1% NPGS +0.5% OV-17+0.5% SE-30(column 2) on chromosorb W HP 100-120 mesh, were used. On the column 1. the nineteen amino acids except histidine were obtained. However, alanine and valine peaks were not separated by this column. On the column 2, the sixteen amino acid peaks showed good separation, but tryptophan. arginine, histidine, and tyrosine peaks were not obtained. Calibration graphs for all amino acids obtained by the plotting the ratios of their peaks hights to that of internal standard versus the micro mole of the amino acids in the range $1.25{\times}10^{-3}{\mu}mol-1.0{\times}10^{-2}{\mu}mole$ showed linearity and passed through the origin.

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Measurement of optical purity for commercial naproxen by chiral HPLC (키랄 크로마토그래피에 의한 시판되는 나프록센의 광학순도 측정)

  • Yu, Jeong-Jae;Lee, Won-Doo;Ryoo, Jae-Jeong
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.360-367
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    • 2011
  • Optical purities of 10 commercialized naproxens prepared from eight Korean drug companies were examined by an optimized chiral HPLC condition. The Chiralcel OD-H column and ChiralHyun-LE(S)-1 column were used as chiral stationary phases and the mixed eluent of hexane/isopropanol/acetic acid as 100:2.85:0.1 was used as a mobile phase for effective enantioseparation. Optical purity values of most samples were higher than 97 percents, only one of them was about 95 percents. The average relative standard deviation of them appeared very small (0.034%).

Measurement of Optical Purity for Commercially Avialable Naproxen Sold in 2013 (2013년 시판된 나프록센의 광학순도 측정)

  • Seo, Hae Chan;Song, Jung Suk;Ryoo, Sang Hyun;Lee, Sang Heon;Ryoo, Dong Hyun;Yu, Jeong Jae;Ryoo, Jae Jeong
    • Journal of the Korean Chemical Society
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    • v.58 no.2
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    • pp.179-185
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    • 2014
  • Commercial (S)-naproxen was racemized under strong basic condition. After checking the peak position of (R)- and (S)-naproxen by analysis the recemized naproxen, optical purity of 19 commercialized naproxens sold in 2013 in Korea were examined by chiral HPLC. The Chiralcel OD-H column, ChiralHyun-LE(S)-1 column and LUX-Cellulose-1 column were used as chiral stationary phases and the mixed eluent of hexane:isopropanol:acetic acid as 100:1:0.1 was used as a mobile phase with a flow rate of 1.0 mL/min. Each data was obtained from an average value of at least three different experiments for each sample and the relative standard deviation of them appeared very small. The average optical purity values obtained from three different chiral columns were very similar and the total average optical purity value (99.32%) of nineteen commercialized naproxens used in this study were larger than those of three years ago (98.17%).

Measurement of Optical Purity for Commercially Avialable Dexibuprofen and Ibuprofen Sold in 2013 (2013년도 시판된 Dexibuprofen과 Ibuprofen의 광학 순도 측정)

  • Ryoo, Sang Hyun;Lee, Sang Heon;Seo, Hae Chan;Song, Jung Suk;Ryoo, Dong Hyun;Yu, Jeong Jae;Kim, Hyun Young;Lee, Jae Hwan;Ryoo, Jae Jeong
    • Journal of the Korean Chemical Society
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    • v.58 no.3
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    • pp.277-282
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    • 2014
  • The optical purity of 11 commercial dexibuprofens and 7 ibuprofens sold in Korea in 2013 were examined by chiral HPLC. The Chiralcel OD-H column and LUX-Cellulose-1 column were used as chiral stationary phases and the mixed eluent of hexane:isopropanol:acetic acid as 100:1:0.1 was used as a mobile phase with a flow rate of 1.0 mL/min. Each data was obtained from an average value of at least three different experiments for each sample and the average value of relative standard deviation of them appeared very small, 0.19%. Average optical purity value (97.5%) of eleven commercial dexibuprofens used in this study were smaller than those of 9 years ago (99.2%), but larger than four years ago (95.6%). Enantiomeric ratios of (R)- and (S)-isomers of seven ibuprofen samples used in this experiment were achieved at about 50:50 which was different with the result (44:56) from four years ago.