• Title/Summary/Keyword: Chromatographic resolution

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Composition Studies on the Aromatic Tobacco Varieties (Nicotiana tabacum L.): 1. Characteristics of Less-Volatile Organic Components. (향끽미종 잎담배 성분조성에 관한 연구 1. 휘발성이 적은 유기성분의 특성조사)

  • Kim, Kyoung-Rae;Park, Jeen-Woo;Lee, Un-Chul;Heu, Il
    • Journal of the Korean Society of Tobacco Science
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    • v.2 no.2
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    • pp.1-7
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    • 1980
  • Less-volatile organic components in leaves from aromatic tobaccos of different varieties, both Oriental and Korean types were isolated and concentrated using a simple apparatus with fewer manipulations. Each less-volatile concentrate was then subjected to spectrophotometric recording in the visible range, to thin-layer chromatographic group separation, and high-performance liquid chromatographic profile analysis. The methods allow detection of significant quantitative differences in visible absorption spectra, TLC patterns, and high resolution HPLC profiles among varieties.

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A Newly Developed Analytical and Semi-preparative Enantiomer Separation of Fluoxetine using Polysaccharide-derived Chiral Stationary Phases by High Performance Liquid Chromatography (고성능 액체 크로마토그래피에 의한 다당 유도체의 키랄 고정상에서 플록세틴의 새롭게 개발된 분석 및 반분취의 광학분리)

  • Kim, Seok Jin;Nam, Kyung Wook;Park, Bohyun;Islam, Md. Fokhrul;Lee, Wonjae
    • KSBB Journal
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    • v.31 no.3
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    • pp.186-191
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    • 2016
  • A liquid chromatographic method for the enantiomer separation of fluoxetine was performed using covalently bonded and coated type polysaccharide-derived chiral stationary phases (CSPs). The degree of enantioseparation is affected by the used CSPs and mobile phases. The performance of Chiralpak IC was superior to the other CSPs used in this study. Out of various solvent composition and additives, the greatest separation and resolution was observed using Chiralpak IC with mobile phase of 2-propanol in hexane with diethylamine as an additive. Semi-preparative separation of fluoxetine was performed on the analytical Chiralpak IC column to obtain (R)- and (S)-fluoxetine enantiomer with high chemical and optical purity. From the overall study, the developed liquid chromatographic method on polysaccharide-derived CSPs is expected to be very useful for the enantiomer separation of fluoxetine.

Solid-Phase Extraction of L-Muscone from Aqueous Samples with Amberlite XAD-4 for Gas Chromatographic Assay

  • Paik, Man-Jeong;Kim, Kyoung-Rae
    • Archives of Pharmacal Research
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    • v.27 no.5
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    • pp.539-543
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    • 2004
  • An efficient analytical method was devised for the accurate L-muscone assay in aqueous samples. It involves solid-phase extraction of L-muscone in adsorption mode using XAD-4 as the sorbent and dichloromethane modified with 10% (v/v) methanol as the eluting solvent. The gas chromatographic analysis of the eluate residue dissolved in toluene on a DB-5MS capillary column provided complete resolution of L-muscone from the co-extracted interferences. The overall method showed excellent linearity ($r^2{\geq}$ 0.9994) in the range of 0.1 to 2.0 $\mu\textrm{g}$/mL with good intra- and inter-day precisions (% RSD = 2.5~7.3) and with high extraction recovery rates ($\geq$ 98.1 %). When the present method was applied to a L-muscone herbal drink product, the within-batch RE (%) in the labeled concentration (1.5 $\mu\textrm{g}$/mL) for the three randomly chosen bottles were -2.4, -1.3 and -3.3 with high precision (% RSD $\leq$ 3.1). The present method is considered to be suitable for quality control evaluation on liquid drinks and other complex formulations fortified with L-muscone.

Reverse-Phase High Performance Liquid Chromatographic Determination of Amino Acids after Precolumn Derivatization with 1-Dimethyl-aminonaphthalene-5-sulfonyl chloride (Dansyl 유도체화와 역상 고성능액체크로마토그래피에 의한 아미노산의 정량)

  • 나혜경;전덕영;홍윤호
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.22 no.6
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    • pp.815-822
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    • 1993
  • This experiment was carried out to determine the separation condition of 1-dimethylaminonaphthalene-5-sulfony(Dansyl) derivatives of amino acids by reverse-phase high performance liquid chromatography with Nova-Pak C18 column. Determined solvent system was solvent A(200mA phosphate buffer pH 6.8 15%, acetonitrile 11%, water 74%) and solvent B(acetonitrile 65%, methanol 28%, water 7%). Linear gradient of solvent B was applied from 12% to 80% for 50min. Complete separation of 20 amino acids including asparagine and glutamine which constitute protein was achieved within 50min. As the detection limit was the range of picomole, the resolution power was excellent. Reproducibility of the retention time was less than mean $\pm$0.05min. According to the above optimum chromatographic conditions, the amino acid composition of some food and human blood was examined. The most affluent amino acid was alanine in human blood, aspartic acid and glutamic acid in soy sauce, alanine and threonine in soy milk and proline in milk and yoghurt.

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Chromatographic Enantiomer Separation and Determination of Optical Purity for α-Amino Acid Esters as 9-Anthraldimine Derivatives Using Polysaccharide Based Chiral Columns (다당 유도체를 기초로 한 키랄 컬럼에서 아미노산 에스테르의 안트르알디민 유도체의 광학분리 및 광학순도 측정)

  • Huang, Hu;Jin, Jing-Yu;Lee, Won-Jae
    • KSBB Journal
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    • v.26 no.2
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    • pp.139-142
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    • 2011
  • The chromatographic enantiomer separation of 9-anthraldimine derivatives of ${\alpha}$-amino acid methyl and ethyl esters on four polysaccharide based chiral columns was performed. The 9-anthraldehyde Schiff base derivatives of ${\alpha}$- amino acid esters were readily synthesized by stirring the ${\alpha}$- amino acid ester hydrochloride salts with 9-anthraldehyde in the presence of 1,8-diazabicyclo [5.4.0]undec-7-ene as a base and anhydrous $MgSO_4$. Chiralcel OD or Chiralcel OD-H showed the greatest enantiomer resolution of 9-anthraldimine derivatives of ${\alpha}$-amino acid methyl and ethyl esters. The L-enantiomers of all the analytes were preferentially retained on Chiralcel OD or Chiralcel OD-H. This analytical method was applied in the determination of optical purities of several commercially available D- or L-${\alpha}$-amino acid methyl esters.

Empirical Equation for Resolution if Ibuprofen Enantiomers by Chiral High-Performance Liquid Chromatography (키랄 고성능 액체 크로마토그래피를 이용하 이부프로펜의 분리도에 관한 실험식)

  • 여미순;노경호
    • KSBB Journal
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    • v.18 no.4
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    • pp.261-265
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    • 2003
  • Ibuprofen was analyzed by chiral high performance liquid chromatography. Retention behaviours of the standard mixtures of ibuprofen were investigated to obtain their acceptable resolution. A chromatographic column (3.9 ${\times}$ 300 mm) was packed by Kromasil CHI-TBB packings (10 $\mu\textrm{m}$) and n-hexane was used as a mobile phase with 0.1% acetic acid and tert-butyl methyl ether. Isocratic elution of ibuprofen at 1.0 $m\ell$/min was performed by changing the mobile phase compositions. The experimental variables affecting the resolution were the compositions of mobile phase and chemical buffer (n-hexane and tert-butyl methyl ether). The resolution between the enantiomers were correlated into the several types of empirical equations including linear form, and their agreements between experimental data and calculated values were examined by the regression coefficient.

Enantiomer Separation of Chiral Amino Alcohols as 9-anthraldimine Derivatives on Coated and Covalently Bonded Chiral Stationary Phases Based on Polysaccharide Derivatives by High Performance Liquid Chromatography (고성능 액체 크로마토그래피에 의한 다당 유도체를 기초로 한 흡착되거나 공유결합된 키랄 고정상에서 키랄 아미노 알코올의 안트르알디민 유도체의 광학분리)

  • Xu, Wen Jun;Jin, Jing Yu;Lee, Won-Jae
    • KSBB Journal
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    • v.26 no.4
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    • pp.323-327
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    • 2011
  • The convenient derivatization method of chiral amino alcohols as 9-anthraldimine Schiff base derivatives for chiral resolution was developed and the liquid chromatographic enantiomer separation of chiral amino alcohols as 9-anthraldimine derivatives was investigated on several coated and covalently bonded polysaccharide-derived chiral stationary phases (CSPs). In general, the performance of Chiralcel OD-H (or Chiralcel OD) (${\alpha}$ = 1.24-2.89), the coated CSP derived from cellulose derivative was superior to the other CSPs for resolution of 9-anthraldimine derivatives of several amino alcohols. The results of enantioseparation depending on the structure of 9-anthraldimine analytes like the steric bulky group and the polar moiety etc were discussed. The analytical method was applied to measure the enantiomeric purity of commercially available chiral amino alcohols. It is expected that the convenient analytical method will be very efficient for determination of enantiomeric purity of amino alcohols as 9-anthraldimine Schiff base derivatives with strong UV absorption.

Alternative Sample Preparation Techniques in Gas Chromatographic-Mass Spectrometric Analysis of Urinary Androgenic Steroids

  • Cho, Young-Dae;Choi, Man-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.9
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    • pp.1315-1322
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    • 2006
  • The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.

Effect of Concentration of Ionic Liquids on Resolution of Nucleotides in Reversed-phase Liquid Chromatography

  • Hua, Jin Chun;Polyakova, Yulia;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.601-606
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    • 2007
  • The chromatographic behaviors of nucleotides (inosine 5'-monophosphate, uridine 5'-monophosphate, guanosine 5'-monophosphate, and thymine monophosphate disodium salts) on a C18 column were studied with different types of ionic liquids (ILs) as additives for the mobile phase in reversed-phase liquid chromatography (RPLC). Three ILs, 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF4]), 1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIm][BF4]), and 1-ethyl-3-methylimidazolium methylsulfate ([EMIm][MS]), were used. Eluents were composed of water and methanol (90/10%, vol) with the addition of 0.5-13.0 mM of ILs. The effects of the concentration of ILs on retention and separation were investigated and discussed. The results showed that the addition of ILs affects the retention and resolution of the tested compounds. Use of 13.0 mM of [BMIm][BF4] as the eluent modifier resulted in a baseline separation of nucleotides without requiring gradient elution. This study demonstrates that ILs can be potentially applied as a mobile phase modifier in RPLC.

Avantor® ACE® UltraCore HPLC and UHPLC Columns (Avantor® ACE® UltraCore HPLC/UHPLC 칼럼 가이드)

  • Peter Bridge;Ian Phillips;Gemma Lo;Cassandra Rusher
    • FOCUS: LIFE SCIENCE
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    • no.1
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    • pp.4.1-4.15
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    • 2024
  • The Avantor® ACE® UltraCore series encompasses High Performance Liquid Chromatography (HPLC) and Ultra High Performance Liquid Chromatography (UHPLC) columns designed to deliver high throughput and high-efficiency ultra-fast separations. Utilizing ultra-inert solid-core silica particles with monodisperse particle distribution, these columns combine the high efficiency of UHPLC with the operability of HPLC instrumentation, yielding lower backpressure and high-resolution separations suitable for a broad spectrum of analytes. The Avantor® ACE® UltraCore range includes three primary product types: • UltraCore BIO: Designed for large biomolecules (≥5 kDa), these columns offer exceptional performance in separating biologically derived compounds. • UltraCore: Ideal for standard small organic molecules, providing rapid separations for both synthetic and natural mixtures. • UltraCore Super: Equipped with encapsulated bonding technology for small organic molecules in extreme pH conditions, optimal for high pH buffer requirements. The Avantor® ACE® UltraCore columns present a versatile and high-efficiency solution for chromatographic separation needs, accommodating a wide range of molecular sizes and providing enhanced resolution and reduced analysis time. Their adaptability to both HPLC and UHPLC systems, combined with the advantages of solid-core technology, makes them an invaluable tool in analytical and preparative chromatography.

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