• Title/Summary/Keyword: Enantiomer separation

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Resolution of Salbutamol Enantiomers in Human Urine by Reversed-phase High Performance Liquid Chromatography after Derivatization with (S)-(-)-${\alpha}$-methylbenzyl isocyanate

  • Kim, Kyeong-Ho;Kim, Tae-Kyun;Kwon, Young-Hee;Sohn, Young-Teak
    • Archives of Pharmacal Research
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    • v.20 no.5
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    • pp.486-490
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    • 1997
  • A stereospecific HPLC method has been developed for the resolution of the enantiomers of salbutamol in human urine. After solid-phase extraction and derivatization with (S)-(-)-${\alpha}$-methyl-benzyl isocyanate, the diastereomeric derivatives were resolved $(R_s=1.59)$ on $5{\mu}M$ octadecylsilan column using 47% methanol as a mobile phase with fluorescence detection. The detection limit of each enantiomer was 10 ng/ml (S/N=3).

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HPLC를 이용한 ketoprofen racemate의 분리

  • Yun, Tae-Ho;Kim, Hyeong-Won;Kim, In-Ho
    • 한국생물공학회:학술대회논문집
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    • 2001.11a
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    • pp.693-696
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    • 2001
  • Ketoprofen racemate is very useful pharmaceutical intermediate, but the hardness of separation to each enantiomer is most a barrier to apply pharmaceutical industry. To overcome this difficulty, we would like to separate S-ketoprofen from ketoprofen racemate. To design suitable mobile phase, hexane and t-BME(tri-buthyl-methyle-ether) were used to elute peaks of ketoprofen racemate separately. When the ratio of hexane/t-BME/acetic acid was 60/40/0.1(%v/v), each component was separated successfully. In order to separate large amount of S-ketoprofen, sample concentration was increased from 100ppm to 2000ppm. In this case, resolution was decreased due to the overlapping of peaks(1.65${\rightarrow}$0.94).

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Resolution of Salbutamol Enantiomers in Human Urine by Reversed-Phase High Performance Liquid Chromatography after Derivatization with 2,3,4,6-Tetra-O-acetyl-${\beta}$-D-glucopyranosyl Isothiocyanate

  • Kim, Kyeong-Ho;Kim, Tae-Kyun
    • Archives of Pharmacal Research
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    • v.21 no.2
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    • pp.217-222
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    • 1998
  • A stereospecific HPLC method has been developed for the resolution of the enantiomers of salbutamol in human urine. After solid-phase extraction and derivatization with 2,3,4,6-tetra-O-acetyl-$\beta$-D-glucopyranosyl isothiocyanate, the diastereomeric derivatives were resolved (Rs=1.83) on $5{\mu}m$ octadecylsilan column using 35% acetonitrile in 0.05M ammonium acetate buffer (pH=6) as a mobile phase with electrochemical detection. The diastereomeric derivatives were formed within 30 min. The detection limit of each enantiomer was 20 ng/ml (S/N=3).

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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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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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    • v.31 no.3
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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.

Chiral Separation of Salbutamol Enantiomers in Human Plasma

  • Seo, Joung-Min;Kim, Kyeong-Ho
    • Archives of Pharmacal Research
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    • v.17 no.4
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    • pp.244-248
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    • 1994
  • A stereoselective and sensitive high performance liquid chromatography using fluoresecence deterctor was examined for the determination of R(-) and S(+)-salbutamol in human plasma. Solid phase extraction method using silica as sorbent was used to extract salbutamol racemates from the plasma matrices. After fractionation and freeze-drying of the eluates containing salbutamol racemates, they were separated and quantified on a chirla stationary column. The detection limit of each enantiomer was 2 ng/ml in human plasma (S/N=3).

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