• Title/Summary/Keyword: Chromatographic factors

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Enantioseparation on HPLC Chiral Stationary Phases

  • Hyun Myung-Ho;Ryoo Jae-Jeong;Min Chung-Sik;William H. Pirkle
    • Bulletin of the Korean Chemical Society
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    • v.13 no.4
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    • pp.407-413
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    • 1992
  • The chromatographic separation of the stereoisomers of the N-(3,5-dinitrobenzoyl) derivatives of fifteen dipeptide methyl esters and nine dipeptide alkyl esters was investigated on three different chiral stationary phases derived from N-acylated ${\alpha}-arylalkylamines$. Two of these CSPs contain second stereogenic centers. These secondary stereogenic centers of CSPs were proposed to provide secondary effects in terms of chiral recognition. From the elution orders of the four dipeptide stereoisomers and the separation factors of the enantiomeric pairs of the N-(3,5-dinitrobenzoyl) derivatives of the dipeptide alkyl esters having different alkoxy substituents, it was proposed that the intercalation of the alkoxy substituents of dipeptide derivatives between the connecting arm of CSPs may control the magnitude of chiral separations of dipeptide derivatives.

Liquid Chromatographic Resolution of Both $\pi$-Acidic and $\pi$-Basic Analytes on a Chiral Stationary Phase Derived from (S)-Tyrosine

  • 현명호;민정식
    • Bulletin of the Korean Chemical Society
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    • v.17 no.12
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    • pp.1117-1123
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    • 1996
  • Chiral recognition models for resolving π-basic N-acyl-α-(1-naphthyl)alkylamines and π-acidic N-(3,5-dinitrobenzoyl)-α-amino alkyl esters on a (S)-tyrosine-derived chiral stationary phase (CSP) containing both π-basic and π-acidic interaction site have been proposed. In the models, the CSP was supposed to interact with the analytes through the π-π interaction between the 3,5-dinitrophenyl or the 3,5-dimethylphenyl group of the CSP and the 1-naphthyl or the 3,5-dinitrophenyl group of the analyte, and through the hydrogen bonding interaction between the appropriate N-H hydrogen of the CSP and the appropriate carbonyl oxygen of the analyte. In this instance, the alkyl substituent of the pertinent enantiomer of the analyte was found to intercalate between the adjacent strands of the bonded phase and consequently control the trends of the separation factors.

Enrichment of Magnesium Isotopes by Monoazacrown Bonded Merrifield Peptide Resin.

  • Kim, Dong Won
    • Bulletin of the Korean Chemical Society
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    • v.22 no.6
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    • pp.570-574
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    • 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.

Reversed-Phase Ion-Interaction Chromatography of Aromatic Sulfonic and Carboxylic Acids (방향족 슬폰산 및 카르복시산의 역상 이온-상호작용 크로마토그래피)

  • Kang Sam-Woo;Oh Hae-Beom;Lee Seung-Seok
    • Journal of the Korean Chemical Society
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    • v.32 no.2
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    • pp.113-121
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    • 1988
  • The retention mechanism and separation of various aromatic sulfonic and carboxylic acids on reversed-phase liquid chromatographic column were studied in the mobile phase containing dodecyltrimethylammonium bromide (DTAB). The retention mechanism was found to be followed the ion-interaction model where the DTAB occupies a primary layer at the stationary phase while the sample anions and other co-anions in the system compete for forming the secondary layer. The capacity factors of samples were influenced by the several factors such as pH, concentration of various organic solvents, co-anions in the mobile phase and functional groups in sample molecules. Some mixtures of organic samples were attempted to separate under optimum condition.

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Resolution of Tocainide and Its Analogues on a Doubly Tethered N-CH3 Amide Chiral Stationary Phase Based on (+)-(18-Crown-6)-2,3,11,12-tetracarboxylic Acid

  • Lee, Kyu Jung;Tak, Kyung Mi;Hyun, Myung Ho
    • Bulletin of the Korean Chemical Society
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    • v.34 no.10
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    • pp.2978-2982
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    • 2013
  • A doubly tethered $N-CH_3$ amide chiral stationary phase (CSP 4) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid was applied to the resolution of an antiarrythmic agent, tocainide, and its analogues and the chromatographic resolution results were compared with those on a singly tethered N-H amide CSP (CSP 1), a singly tethered $N-CH_3$ amide CSP (CSP 2) and a doubly tethered N-H amide CSP (CSP 3) under an identical aqueous mobile phase condition. CSP 4 was found to be generally better than other CSPs in terms of the separation factors (${\alpha}$) and resolutions (RS). The retention times of analytes denoted by the retention factors ($k_1$) on CSP 4 were quite long compared to those on other CSPs because of the improved lipophilicity of CSP 4. The long retention times of analytes on CSP 4 were successfully controlled by the addition of a small amount of ammonium acetate to aqueous mobile phase without hurting the chiral recognition efficiency. The variation of the content and type of organic and acidic modifier in aqueous mobile phase was found not to change the chiral recognition efficiency significantly.

Reversed-Phase Liquid Chromatographic Separation of Metal Ions by Chelate Formation with 1-(2-Pyridylazo)-2-Naphthol (역상 액체크로마토그래피에 의한 1-(2-Pyridylazo)-2-Naphthol과 킬레이트를 형성하는 금속이온의 분리)

  • Kang, Sam Woo;Park, Sun Ja
    • Journal of the Korean Chemical Society
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    • v.42 no.2
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    • pp.197-202
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    • 1998
  • 1-(2-Pyridylazo)-2-Naphthol (PAN) has been widely used as a spectrophotometric reagent and metallochromic indicator for many metal ions. In this work, the chelate reagent of PAN was used as mobile phase additive for the separation of metal ions by reversed phase chromatography. Metal ions could be detected by monitoring the effluent at 570 nm with spectrophotometric detector. In order to investigate retention behaviors of the metal ions, the chromatograms and capacity factors were obtained as the variation of pH, ionic strength and composition of organic modifier in mobile phase. Under the obtained optimum conditions, the mixtures of Fe(III), Ni(II), Cu(II), Zn(II) and Co(II) could be separated successfully and the calibration curves under the recommended conditions showed an excellent linearity. The detection limits(S/N) were feasible at the nanogram level.

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Comparative Analyses of the Flavors from Hallabong (Citrus sphaerocarpa) with Lemon, Orange and Grapefruit by SPTE and HS-SPME Combined with GC-MS

  • Yoo, Zoo-Won;Kim, Nam-Sun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.271-279
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    • 2004
  • The aroma component of Hallabong peel has been characterized by GC-MS with two different extraction techniques: solid-phase trapping solvent extraction (SPTE) and headspace solid-phase microextraction (HSSPME). Aroma components emitted from Hallabong peel were compared with those of other citrus varieties: lemon, orange and grapefruit by SPTE and GC-MS. d-Limonene (96.98%) in Hallabong was the main component, and relatively higher peaks of cis- ${\beta}$-ocimene, valencene and -farnesene were observed. Other volatile aromas, such as sabinene, isothujol and ${\delta}$-elemene were observed as small peaks. Also, principal components analysis was employed to distinguish citrus aromas based on their chromatographic data. For HSSPME, the fiber efficiency was evaluated by comparing the partition coefficient ($K_{gs}$Kgs) between the HS gaseous phase and HS-SPME fiber coating, and the relative concentration factors (CF) of the five characteristic compounds of the four citrus varieties. 50/30 ${\mu}$m DVB/CAR/PDMS fiber was verified as the best choice among the four fibers evaluated for all the samples.

Separation of Functionalized Heterocyclic Compounds by High Performance Liquid Chromatography (II) (고성능 액체 크로마토그래피에 의한 기능성 헤테로 고리 화합물의 분리(II))

  • Cho, Yun Jin;Lee, Young Cheol;Lee, Kwang-PiII;Park, Keung-Shik
    • Analytical Science and Technology
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    • v.11 no.4
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    • pp.292-296
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    • 1998
  • Normal phase or reversed phase liquid chromatographic separation of isoquinoline of heterocyclic compounds and structural isomers of external substituents, $COOCH_3$, CN and $CH_3$ has been carried out by using several different columns and various mobile phases. From this results, the order of elution of heterocyclic compounds appears to depend on the solvent effect with kinds of mobile phases. Retention mechanism of normal phase system for 2-methylindoline, 2-methylindole, benzoxazole and benzothiazole was also studied depending on adsorption strength between solute and stationary phase of column. However, retention factors of reversed phase system were found on hydrophobic interaction with solvophobic effect.

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Studies on the Population of Toxigenic Fungi in Foodstuffs(VIII) (한국 식품중의 유독성 진균에 관한 연구 8)

  • Koh, Choon-Myung;Kim, Se-Jong;Cho, She-Hoon;Kim, Sung-Kwang;Lew, Joon
    • Korean Journal of Microbiology
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    • v.12 no.2
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    • pp.59-68
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    • 1974
  • With an aim to disclose causal factors scably grains intoxications, the screening of toxic Fusaria and the detection of toxic priniciples were performed in respect of cultured cells bioassay with HeLa cells, skin-necrotizing effect, histopathological investigation and also chromatographic analysis sith following results ; 1. Among the fungi, Fusarium sp. F-27, F-63 and F-61 were highly toxic to mice, causing liver injury characterized necrosis and inflammation. 2. HeLa cell culture bioassay demonstrated that the cell of the isolated strains of Fusaria were suspected to produce toxic material (Fusarenon-X). 3. The culture filtrates of Fusarium nivale Fn-2B, F-27, and F-63, were injected subcutaneously, and caused inflammation followed by crust on the skin ICR-mice. 4. The observation method of skin-necrotizing effect to the mice can be used to the screening to the toxin-producing fungi isolated from many fusarial contaminations.

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Statistical Analysis on the Sources of Variance in Proficiency Test of Quantitative Analysis of Medicines (의약품 함량분석 정도관리에서의 변이 요인에 대한 통계분석)

  • Cho, Jung-Hwan
    • Journal of Pharmaceutical Investigation
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    • v.37 no.1
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    • pp.27-37
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    • 2007
  • Proficiency test is an essential tool far ensuring analytical ability of analytical chemists and analytical institutes. Usually, the standard protocol for proficiency test is focused on acceptability of reported analytical results of participants by calculating z-scores and related diagnostic parameters. The ultimate goal of this process is to reveal the sources of variability of analytical results and to find the way to reduce their influence. In this study, the method of analysis of variance (ANOVA) was applied to the analytical data collected from qualify control departments of pharmaceutical companies in KyungIn province in Korea in the year of 2000. As influencing factors of variability of analytical results, the use of internal standards for liquid and gas chromatograpy, the educational and professional background of participants, geological locations and yearly production sizes of participating companies were evaluated. To evaluate the variability in accuracy of analytical results, absolute differences from sample mean and sample median were used and to evaluate variability in precision of individual participants, the reported standard deviation of each participant was used. As a result, the use of internal standards in gas chromatographic analysis, participants' academic background and the yearly production sizes of pharmaceutical companies showed statistically significant influence to the accuracy and the precision of the reported analytical results used in this study.