• Journal of the Korean Chemical Society
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• v.33 no.3
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• pp.287-294
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• 1989

The optimum condition for the separation of priority pollutant phenols using isocratic elution has been determined. The elution behavior of eleven phenols has been also studied to interpret the retention. The reversed phase liquid chromatographic methods were performed on a ${\mu}$-Bondapak $C_{18}$ column with methanol-water, acetonitrile-water, and THF water mixtures as mobile phases. The COF method, where Snyder's solvent triangle concept was combined with a mixture-design statistical technique, was used to optimize the strength and selectivity of solvents for the separation of phenols. The optimum solvent composition, which gives a complete separation of eleven phenols, was found to be $MeOH:ACN:H_2O$ = 7:40:53. The plots of ln k' vs. -${\Delta}H^{\circ}$ and ${\Sigma}{\pi}$ of phenols showed relatively good linearities. Effect of van der Waals volume, pi-energy and hydrogen bonding on the retention of phenols were investigated. The following equation with the correlation coefficient of 0.9927 for ACN-water solvent system was obtained; $log^{k'}=2.515{\times}10^{-2}VWV-1.301{\times}10^{-1}E-3.674{\times}10^{-1}$

• Analytical Science and Technology
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• v.7 no.1
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• pp.25-31
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• 1994

As for analytes which did not represent the differences of the selectivity on the stationary and mobile phase, secondary chemical equilibrium theory was applied to study pH effects on the separation of alkylphenols. Mobile phase was consisted of an aqueous sodium carbonate-bicarbonate buffer and acetonitrile. The maximum selectivity for adjacent peak pairs was predicted from those values of $k^{\prime}_{HA}/k^{\prime}_{A-}$ and ${\Delta}pK$. The optimum pH determined by this method was 11.18 pH and solvent selectivity were considered at the same time to invoke the full range of selectivity effects possible for separations. Quaternary mixture composed of methanol, acetonitrile, tetrahydrofuran and water was adjusted to optimum pH 11.18. As the statistical simplex technique of an overlapping resolution map (ORM) was used to predict the optimized solvent system. The optimum solvent, which gives complete separation of alkylphenols, was determined as follws MeOH : ACN : THF = 14.4 : 81.8 : 2.8.

• 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.

• Analytical Science and Technology
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• v.5 no.4
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• pp.389-399
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• 1992

Liquid Chromatographic behavior of Pd(II) in Isonitrosoethylacetoacetate lmine, $Pd(IEAA-NR)_2$ (R=H, $CH_3$, $C_2H_5$, $n-C_3H_7$, $C_6H_5-CH_2$, $n-C_4H_9$) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of $Pd(IEAA-NR)_2$ chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It wass found that metal chelates were properly eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the logarithm of capacity factor(k') on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extration distribution ratio($D_c$) in methanol-water/n-alkane extration system was investigated. Both kinds of dependence are linear, which susggests that the retention of the electroneutral metal chelate is largely due to the solvophobic effect. Standard adsorption enthalpy changes (${\Delta}H^{\circ}$) and standard adsorption entropy changes (${\Delta}S^{\circ}$) of Pd(II) Isonitrosoethylacetoacetate imine chelates on Micropak MCH-5 column were calculated by measuring capacity factor with changing temperature of the column.

• Journal of the Korean Chemical Society
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• v.36 no.5
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• pp.697-708
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• 1992

Liquid Chromatographic behavior of Ni(II) in Isonitrosoethylacetoacetate Imine(IEAA-NR), Ni(IEAA-NH)(IEAA-NR)(R = H, CH_3, C-2H_5, n-C_4H_9, C_6H_5-CH_2) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of Ni(IEAA-NH)(IEAA-NR) chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It was fo$und that metal chelates were properly eluted in an acceptable range of capacity factor value(0{\le}logk'{\le}1). The dependence of the logarithm of capacity factor (k') on the volume fraction of water in the binary mobile phase as well as on the liquid-liquid extraction distribution ratio (Dc) in methanol-water/n-alkane extraction system showed the good linearties, and the dependence of the logarithm of capacity factor (k') on the column temperature and on the enthalpy exhibited the good linearties, and the compensation temperature ({\beta}) from the slope was 773.47{\circ}K. It was suggested that the retention of metal chelates was largely affected by the hydrophobic effect.

• Journal of Food Hygiene and Safety
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• v.11 no.2
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• pp.149-157
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• 1996

A procedure for the determination of Aflatoxins in food and grains which utilizes reversed phased liquid chromatographic (LC) analysis with postcolumn derivatization by an electrochemical cell and determination with a fluorescence detector has been evaluated. The LC mobile phase was water-acetonitrile-methanol (6+2+2) with 1mM KBr and 1 mM HNO3 which gave baseline separation for the four Aflatoxins (AfB1, AfB2, AfG1, AfG2). The electrochemical cell set at 7V, generated bromine and derivatized aflatoxins B1 and G1, The derivatives were detected by the fluorescence detector. The aflatoxins in naturally contaminated corn samples were isolated by three different cleanup procedures: the AOAC method I column(CB method), a rapid filtrate column (Romer's column), and an immunoaffinity column. The final extract were quantitated with fluordensitometric TLC and the LC postcolumn derivatization techniques. The results were quite similar, however the LC technique showed less interferences and could be automated. Samples of corn, raw peanuts, peanut butter and dried dates were also analyzed successfully with this procedure.

• The Korean Journal of Food And Nutrition
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• v.20 no.2
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• pp.125-133
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• 2007

Ginger(Zingiber officinale Roscoe) has long been used as a food source in Korea, and it is widely used as a dietary condiment throughout the world. The present study focused on the immunomodulative effects of ginger extracts via in vitro experiments. To identify the immune-activation fractions of the plant, we performed the systematic fractionation of ginger with methanol, hexane, chloroform, butanol and water for separation and refining. The results showed that the chloroform fraction had the highest immune cell activation properties. In conclusion, this study suggests that ginger extracts may enhance immune function by regulating the splenocyte proliferation as well as the cytokine production capacity of activated macrophages.

• Archives of Pharmacal Research
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• v.22 no.6
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• pp.608-613
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• 1999

Optimum conditions of chiral derivatization reaction of $\beta$-blockers (acebutolol, arotinolol, betaxolol, bisoprolol, celiprolol, metoprolol and pindolol) with (-)-menthyl chloroformate were investigated for the resolution by HPLC. With more than 30 times molar excess of (-)-methyl chloroformate chiral derivatization reactions were completed within one hour at room temperature except arotinolol and celiprolol. Diastereomeric derivatives of $\beta$-blockers were well resolved on the ODS column using acetonitrile-methanol-water as a mobile phase.

• Proceedings of the PSK Conference
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• 2002.10a
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• pp.394.2-394.2
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• 2002

A sensitive and selective reversed-phase LC-ESI-MS method to quantitate pseudoephedrine in human plasma was developed and validated. Phenacetin was used as an internal standard. Samples were prepared simply by acetonitrile precipitation without an evaporation step. Chromatographic separation was achieved on a XTerra MS C18 column ($150{times}2.1$ mm I.D.. 3.5 $\mu\textrm{m}$ particles). using gradient elution with 0.5% (v/v) trifluoroacetic acid (TFA) in water and 0.5% (v/v) TFA in methanol at a flow-rate of 0.1 ml/min. (omitted)

• Proceedings of the PSK Conference
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• 2003.04a
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• pp.283.1-283.1
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• 2003

This study was designed to develop and validate an isocratic reversed phase high performance liquid chromatographic(HPLC) method for the quantitation of sobrerol in drug preparations, and obtain the data pool that can be used in the revision of pharmacopoeia. The separation of sobrerol and the other compounds (S-carboxymethylcysteine, acetaminophen, methyl paraben, propyl paraben, and sobrerol degradants) was achieved in a C18 column with an acetonitrile-methanol-water(24.5:10.5:65.0) mobile phase. (omitted)