• Title/Summary/Keyword: Chromatographic retention

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Separation of Positional Isomers in a Calix[4]arene-methylsiloxane Polymer as Stationary Phase in Capillary GC

  • Seo, Jeong Gi;Kim, In Hwan;Jang, Seung Hyeon;Kim, Byeong Ok;Ryu, Jae Uk;Park, Jeong Hak
    • Bulletin of the Korean Chemical Society
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    • v.22 no.4
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    • pp.409-412
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    • 2001
  • Poly(p-tert-butyltrimethoxymonopropyloxycalix[4]arene-methylsiloxane) (TBCX-MS) has been prepared and used as a stationary phase in isothermal capillary gas chromatographic separation of some positional isomers. Retention factors (k) and separatio n factors $(\alpha)$ for the isomers were measured and compared with those on poly(p-tert-butyl-dimethoxydipropyloxycalix[4]arene-tetramethyldisiloxane) (TBCX-TMDS), poly(dimethoxydipropyloxycalix[4]arenetetramethyl-disiloxane) (CX-TMDS). Most of the isomers investigated are well resolved on TBCX-MS. Retention of all the compounds decreases on the three phases in the order, TBCX-TMDS ${\geq}$ TBCX-MS > CX-TMDS. Similar retention values on TBCX-TMDS and TBCX-MS seem to indicate that retention property of the two phases is not significantly affected by the spatial position of the calixarene moiety.

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

  • Kim, Hee-Jin;Choi, Hee-Jung;Hyun, Myung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.31 no.3
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    • pp.678-682
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    • 2010
  • A doubly tethered chiral stationary phase (CSP) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid were applied to the liquid chromatographic resolution of racemic tocainide, an antiarrhythmic agent, and its analogues. The chiral recognition efficiency of the doubly tethered CSP for tocainide and its analogues was generally greater than that of the corresponding singly tethered CSP especially in terms of the resolution ($R_S$). The resolution of tocainide and its analogues on the doubly tethered CSP were dependent on the content and the type of the organic and acidic modifiers in aqueous mobile phase and the column temperature. Especially, the retention behaviors of analytes on the doubly tethered CSP with the variation of the content of organic modifier in aqueous mobile phase were opposite to those on the corresponding singly tethered CSP and these opposite retention behaviors were rationalized by the lipophilicity differences of the two CSPs.

Chromatographic Behavior of Proteins on Stationary Phase with Aminocarboxy Ligand

  • Li, Rong;Ju, Ming-Yang;Chen, Bin;Sun, Qing-Yuan;Chen, Guo-Liang;Shi, Mei;Wang, Xiao-Gang;Zheng, Jian-Bin
    • Bulletin of the Korean Chemical Society
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    • v.32 no.2
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    • pp.590-594
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    • 2011
  • An aminocarboxy aspartic acid-bonded silica (Asp-Silica) stationary phase was synthesized using L-aspartic acid as ligand and silica gel as matrix. The standard protein mixtures were separated with prepared chromatographic column. The effects of solution pH, salt concentration and metal ion on the retention of proteins were examined, and also compared with traditional iminodiacetic acid-bonded silica (IDA-Silica) column. The results show that Asp-Silica column exhibited an excellent separation performance for proteins. The retention of proteins on Asp-Silica stationary phase was consistent with electrostatic characteristic of cation-exchange. The stationary phase displayed typical metal chelate property after fixing copper ion (II) on Asp-Silica. Under competitive eluting condition, protein mixtures were effectively isolated. Asp ligand showed better ion-exchange and metal chelating properties as compared with IDA ligand.

Optimum Condition of HPLC by HCI Program (HCI 프로그램을 이용한 HPLC의 최적화 조건)

  • Jin, Chun Hua;Lee, Ju Weon;Row, Kyung Ho
    • Korean Chemical Engineering Research
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    • v.44 no.6
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    • pp.555-562
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    • 2006
  • Recently, liquid chromatography (LC) has been used more frequently to separate drugs and natural substances. Especially, to selection of the solutes from the products, the operation condition of analytical chromatography should be necessarily determined. So accurate computer modeling and simulation of chromatographic performances has become a necessary part of the development and design of processes. High-Purity Separation Lab. Inha University developed the resulting HCI software for the purpose of the optimization of chromatographic performances. The HCI program was utilized to find the optimum operating condition more accurately and rapidly, reducing the number of many possible experiments. The elution profiles were calculated by the plate theory based on the three retention mechanism of capacity factor.

Chromatographic Selectivity of Cyano-Bonded Silica Columns in RPLC Based on the Linear Solvation Energy Relationships

  • Park, Jung-Hag;Jang, Myung-Duk;Kwon, Se-Mok
    • Bulletin of the Korean Chemical Society
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    • v.13 no.1
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    • pp.75-79
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    • 1992
  • Differences in chromatographic properties in RPLC of four brands of cyano bonded silica stationary phases are rationalized in terms of the type and relative strength of the solute-stationary phase interactions, which can be readily inferred from multiple linear regression analyses of retention data for a set of standard compounds on the stationary phases under study based on the linear solvation energy relationships (LSERs). Although four brands of cyano bonded columns studied (CPS-Hypersil, Ultrasphere cyano, Spherisorb-CN and ${\mu}$-Bondapak-CN) have similar bonding density and have been prepared from monofunctional cyanopropylsilane reagents, they possess quite different, relative hydrogen bonding (HB) donor and acceptor strengths. Comparison of the retention behavior on a cyano-bonded silica column with that on an ODS column shows that there are significant differences in the strength of HB interactions between the solute and the stationary phase on the two columns with different functionalities. Information on the differences in the interaction characteristics among brands of the cyano-bonded silica columns and between the ODS and cyano-bonded columns can be utilized to optimize the selectivity for a given separation on these columns.

Thermodynamic Properties of the Solute Transfer from the Aqueous Acetonitrile Mobile Phase to the Stationary Phase Monitored by HPLC

  • Jeong, Won Jo;Kim, Ji Yeon;Gu, Yun Mo
    • Bulletin of the Korean Chemical Society
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    • v.21 no.1
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    • pp.105-109
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    • 2000
  • High-performance liquid chromatography is suitable for getting thermodynamic information about solute-solvent interactions. We used a squalane impregnated $C_{18}$ phase as a presumably bulk-like stationary phase to secure a simple partition mechanism for solute retention in reversed phase liquid chromatographic system. We measured retention data of some selected solutes (benzene, toluene, ethylbenzene, propylbenzene, butylbenzene, phenol, benzylalcohol, phenethylalcohol, benzylacetone, acetophenone, benzonitrile, benzylcyanide) at 25, 30, 35, 40, 45, and 50 $^{\circ}C$ in 30/70, 40/60, 50/50, 60/40 and 70/30 (v/v%) acetonitrile/water eluents. The van't Hoff plots were nicely linear, thus we calculated dependable thermodynamic values such as enthalpies and entropies of solute transfer from the mobile phase to the stationary phase based on more than four retention measurements on different days (or weeks). We found that the cavity formation effect was the major factor in solute distribution between the mobile and stationary phases in the system studied here. Our data were com-pared with some relevant literature data.

Volatile Retention during Freeze Drying of Fruit Juices (과실쥬스의 동결건조 중 휘발성분 보유력)

  • 심기환;최진상;주옥수;강갑석
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.19 no.6
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    • pp.555-564
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    • 1990
  • The headspace gas chromatographic(analytical) technique was used to evaluate the retention of volatiles in fruit juices during freeze drying as a function of freezing rate, the content of initial solid and chamber pressure. The effects of freezing rate and drying time on the volatile retention under the experimental conditions were marked, particulary at long freezing time. The retention of volatiles in the freeze dried was largely affected by the freezing rate. The highest volatile loss under the freeze drying conditions was observed during the first stage of drying. The behavior during freeze drying of the volatile substances was affected by high content of initial solid. The volatile retention was higher in quick freeze drying than slow freeze drying and low pressure than high.

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Effect of Eluent Electrolyte on the Retention Behavior of Structural Isomers of Phenols in HPLC. (HPLC 에서 페놀류의 구조 이성질체의 머무름 거동에 대한 전해질 용리액의 효과)

  • Lee, Seon Haeng;O, Dae Seop;Park, Gi Ho
    • Journal of the Korean Chemical Society
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    • v.34 no.1
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    • pp.44-50
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    • 1990
  • The liquid chromatographic retention behavior of structural isomers of phenols was investigated by a change of the mobile phase properties. The retention behavior of structural isomer of phenols in reversed phase liquid chromatography was affected by eluent electrolyte added. It can be seen that this behavior is illustrated by a mechanism of Langmuir isotherm and ion exchange between phenolate and the reversed phase coated with ions. The retention behavior was represented as two different areas according to the concentration of the electrolytes. These areas can be explained as counter ion and co-ion effect, respectively. The maximum retention values were dependent not upon the kinds of organic modifier but upon the kinds of electrolyte.

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Determination of Mono- and Oligosaccharides Derivatized with p-Aminobenzoic Ethyl Ester by Reverse Phase HPLC

  • Kwon, Hyokjoon;Kim, Joon
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.859-864
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    • 1995
  • Mono- and oligosaccharides are derivatized with p-aminobenzoic ethyl ester (ABEE), strongly absorbs UV light at 254 nm, in the presence of sodium cyanoborohydride. C18-bonded silica column is used for the separation of sugar-ABEE derivatives in an isocratic mode. RP-HPLC conditions are optimized by using ternary mixture as mobile phase and $45^{\circ}C$ as a column temperature. Sugar-ABEE derivatives are separated well within a short run time (ca. 25 min) by reverse-phase partition chromatographic mode. The ($1{\rightarrow}6$) linkage type of dihexose-ABEE derivatives has shorter retention time than ($1{\rightarrow}4$)-linkage type. After acid hydrolysis of glycoproteins with 2M trifluoroacetic acid, monosaccharide composition and contents are determined. This procedure is very useful for the simultaneous analysis of neutral and amino sugars in a single chromatographic step using RP-HPLC without reacetylation of deacetylated amino sugars, which are produced by acid hydrolysis.

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Chromatographic Separation of Some Phenol Derivatives Using $\alpha$-Cyclodextrin in Mobile Phase ($\alpha$-씨클로덱스트린을 이동상으로 사용한 몇 가지 페놀 유도체들의 크로마토그래피적 분리)

  • 문영자;김봉희
    • Environmental Analysis Health and Toxicology
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    • v.12 no.3_4
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    • pp.75-84
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    • 1997
  • Chromatographic retention behavior and separation of various phenol derivatives on a Partisil 10 ODS 3 column-with mobile phase containing $\alpha$-cyclodextrin-were systematically studied. The decrease in k' values caused by the addition of cyclodextrins in the mobile phase was based on the formation of an inclusion complex, resulting in weakening of the hydrophobic interaction between solutes and the stationary phase. The content of the organic solvent in the mobile phase also influenced k' values of the solutes, and k' values increased with a decrease of the content of organic solvent in the mobile phase. A simple equation has been derived that reveals the hyperbolic dependence of the capacity factor on the total concentration of cyclodextrin. A plot of the reciprocal of the capacity factor against (CD)$_T$ gives a straight line and the dissociation constant, K$_D$, of the inclusion complex can be calculated from the slope. The capacity factor decreased with increasing temperature. The enthalpy was calculated from the slope of van't Hoff plots. Under optimum conditions, some mixtures of phenol derivatives were able to separated successfully.

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