• Bulletin of the Korean Chemical Society
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• v.34 no.6
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• pp.1745-1750
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• 2013

A novel green aqueous mobile phase modified with room temperature ionic liquids (RTILs) was employed in the absence of volatile organic solvents or ion-pairing reagents to analyze thiamine, a very polar compound, by reverse phase high performance liquid chromatography (RP-HPLC). Due to its strongly hydrophilic nature, thiamine was eluted near the column dead time ($t_0$) using a mobile phase without adding RTILs or ion-pairing reagents, even if a 100% aqueous mobile phase, which has weak elution power under reverse phase conditions, was used. Thus, 1-ethyl-3-methyl-imidazolium hexafluorophosphate ([EMIM][$PF_6$]), which has the strongest chaotropic effect, was selected as a mobile phase additive to improve retention and avoid baseline disturbances at $t_0$. Various mobile phase parameters such as cation moiety, chaotropic anion moiety, pH and concentration of RTILs were optimized to determine thiamine at the proper retention time. Method validation was performed to assess linearity, intra- and inter-day accuracy and precision, recovery and repeatability; all results were found to be satisfactory. The developed method was also compared to the current official United States Pharmacopoeia (USP) and Korean Pharmacopoeia (KP) methods using an organic mobile phase containing an ionpairing reagent by means of evaluating various chromatographic parameters such as the capacity factor, theoretical plate number, peak asymmetry and tailing factor. The results indicated that the proposed method exhibited better efficiency of thiamine analysis than the official methods, and it was successfully applied to quantify thiamine in pharmaceutical preparations.

• Analytical Science and Technology
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• v.9 no.3
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• pp.292-301
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• 1996

The synthesis of poly(ether)tailed bipyridine complex as redox reaction probes has advanced attempts to interpret very slow diffusion and heterogeneous electron transfer. Diffusion coefficients as low as $1.5{\times}10^{-15}cm^2/s$ have been observed for the oxidation of neat $Co(bpy(ppgm)_2)_{3^-}(ClO_4)_2$ with $LiClO_4$ electrolyte. Heterogeneous electron transfer rate constants of materials were found to vary with diffusion coefficient. The decrease in k as the diffusion coefficient decreases was actually caused by the decreasing D. Diffusion coefficient for compound of strong ion pairing anion($ClO{_4}^-$) was much smaller than the diffusion coefficient for compound of weak ion pairing anion($CF_3COO^-$).

• Preventive Nutrition and Food Science
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• v.4 no.3
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• pp.171-174
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• 1999

For monitoring lipid oxidation development in cooked ground pork during refrigerationm, malonaldehydethiobarbituric acid(MA-TBA) contents were measured using high performance liquid chromatography(HPLC). As the oxidation proceeded during refergeration, TBA-reaction substances(TBARS) absorbances increased and the corresponding HPLC peak areas also increased proportationately. The correlation coefficient between the HPLC peak areas and MA-TBA absorbance were 0.9979. The treatemtn of cetrimide, an ion pairing agent, gave a complete resolution of the MA-TBA complex and the butanol extraction of the complex increased its recovery by 37.8%. Both cetrimide treatment and butanol extraction are essential steps for analyzing MA-TBA complex in ground pork wiht HPLC. A reliable and specific measurement of NA-TBA in ground pork was successfully performed using HPLC.

• Bulletin of the Korean Chemical Society
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• v.29 no.1
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• pp.117-121
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• 2008

Pseudo-first-order rate constants (kobsd) have been measured spectrophotometrically for nucleophilic substitution reactions of 5-nitro-8-quinolyl benzoate (5) with alkali metal ethoxides, EtO?M+ (M+ = Li+, Na+ and K+) in anhydrous ethanol (EtOH) at 25.0 0.1 C. The plots of kobsd vs. [EtO?M+] exhibit upward curvatures, while the corresponding plots for the reactions of 5 with EtO?Na+ and EtO?K+ in the presence of complexing agents, 15-crown-5-ether and 18-crown-6-ether are linear with rate retardation. The reactions of 5 with EtO?Na+ and EtO?Li+ result in significant rate enhancements on additions of Na+ClO4, indicating that the M+ ions behave as a catalyst. The dissociated EtO and ion-paired EtOM+ have been proposed to react with 5. The second-order rate constants for the reactions with EtO (kEtO) and EtOM+ (kEtOM+) have been calculated from ion-pairing treatments. The kEtO and kEtOM+ values decrease in the order kEtONa+ > kEtOK+ > kEtOLi+ > kEtO, indicating that ion-paired EtOM+ species are more reactive than the dissociated EtO ion, and Na+ ion exhibits the largest catalytic effect. The M+ ions in this study form stronger complex with the transition state than with the ground state. Coordination of the M+ ions with the O and N atoms in the leaving group of 5 has been suggested to be responsible for the catalytic effect shown by the alkali metal ions in this study.

• Carbon letters
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• v.10 no.4
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• pp.305-313
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• 2009

In this study, the adsorption of toxic pollutants onto cetyltrimethylammonium kaolin (CTAB-Kaolin) is investigated. The organo-kaolin is synthesized by exchanging cetyltrimethylammonium cations (CTAB) with inorganic ions on the surface of kaolin. The chemical analysis, the structural and textural properties of kaolin and CTAB-kaolin were investigated using elemental analysis, FTIR, SEM and adsorption of nitrogen at $-196^{\circ}C$. The kinetic adsorption and adsorption capacity of the organo-kaolin towards o-xylene, phenol and Cu(II) ion from aqueous solution was investigated. The kinetic adsorption data of o-xylene, phenol and Cu(II) are in agreement with a second order model. The equilibrium adsorption data were found to fit Langmuir equation. The uptake of o-xylene and phenol from their aqueous solution by kaolin, CTAB-kaolin and activated carbon proceed via physisorption. The removal of Cu(II) ion from water depends on the surface properties of the adsorbent. Onto kaolin, the Cu(II) ions are adsorbed through cation exchange with $Na^+$. For CTAB-kaolin, Cu(II) ions are mainly adsorbed via electrostatic attraction with the counter ions in the electric double layer ($Br^-$), via ion pairing, Cu(II) ions removal by the activated carbon is probably related to the carbon-oxygen groups particularly those of acid type. The adsorption capacities of CTAB-kaolin for the investigated adsorbates are considerably higher compared with those of unmodified kaolin. However, the adsorption capacities of the activated carbons are by far higher than those determined for CTAB-kaolin.

• Journal of the Korean Chemical Society
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• v.42 no.4
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• pp.416-421
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• 1998

In the reversed-phase ion-pair high performance liquid chromatographic (RPIP-HPLC) elution behavior of noble metal-thiacrown ether complexes, the effects of the concentration of ion-pairing reagent and kind of ligands were studied. It was found that the less the number of atoms in the ring of the thiacrown ether molecule was, the larger the selectivity was, and the elution mechanism of the complexes was explained due to the formation of ion-pair when the concentration of sodium dodecyl sulfate (SDS) in mobile phase was lower than 10 mM and due to the formation of micelle when the SDS concentration was higher than 10 mM. As a conclusion, separations of the noble metal-thiacrown ether complexes in an optimum separation condition were accomplished successfully and the method was proved to be an useful one for the separation and determination of Ag (Ⅰ) ion in a black-white photographic fixing solution.

• Korean Journal of Optics and Photonics
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• v.12 no.3
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• pp.205-211
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• 2001

We propose a constant inversion black box model of erbium-doped fiber amplifiers (EDFAs) for exact performance predictions for EDFAs operated in the gain-flattened condition. The validity of the newly proposed model was experimentally verified by predicting the performance of EDFAs for the L band, within 1.9% required pump power discrepancy. The role of ion pairing effects on the power conversion efficiency is also discussed. ussed.

• Analytical Science and Technology
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• v.12 no.3
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• pp.203-208
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• 1999

The ion-pair high performance liquid chromatographic elution behavior of salicylic acid and its derivatives was studied with measuring capacity factor, k', changing the concentration of ion-pairing reagent (tetrabutylammonium chloride, TBACl) in mobile phase. As a result, it was found that k' of the samples increase at pH 7.2 as the TBACl concentration increases. The derivatives of salicylic acid were separated each other at an optimum mobile phase condition which was found from the observation of the retention behavior. The optimum mobile phase condition was methanol solution($MeOH:H_2O_2$ 30:70) containing 20 mM TBACl for the determination of salicylic acid and methanol solution($MeOH:H_2O_2$ 20:80) containing 40 mM TBACl for p-aminosalicylic acid at pH 7.2. The method has been applied for the analysis of the contents of salicylic acid derivatives in an aspirin tablet and a tuberculosis curing agent.

• Preventive Nutrition and Food Science
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• v.4 no.3
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• pp.167-170
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• 1999

Various concentrations of malonaldehyde (MA) produced upon hydrolysis of 1, 1, 3,3-tetraethoxypropane (TEP) were reacted with 2-thiobarbituric acid (TBA)and th e contents of MA-TBA complex were measured both with spectrophotometer and high performance liquid chromatography (HPLC). As the concentrations of MA-TBA increased, their absorbances and the corresponding HPLC peak areas increased. The correlation coefficient between absorbances and HPLC peak areas of MA-TBA peaks from the other compounds and butanol extraction of the complex increased its recovery its recovery by 29.4% . Measurement of the content of MA-TBA complex for monitoring the development of lipid oxidation was proven to be successful with the use of high performance liquid chromatography.

• Bulletin of the Korean Chemical Society
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• v.13 no.3
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• pp.240-245
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• 1992

The effect of the addition of sodium dodecyl sulfate (SDS) to a buffered mobile phase (pH 3.4) on the retention of nucleotides, nucleosides and bases was investigated with a polyvinyl alcohol (PVA) column. Depending on the concentration of SDS, two different trends in the retention of nucleosides and bases containing an $NH_2$ group were observed. If the concentration of SDS was less than 5.5 mM, the retention of compounds containing an $NH_2$ group increased as the concentration of SDS in the mobile phase increased. In contrast, if the concentration was greater than 5.5 mM, the retention of compounds containing an $NH_2$ group decreased. Thus, the SDS acted as an ion-pairing reagent at lower concentration but formed micelles at higher concentrations. The retention behavior of the nucleosides and bases in the presence of a micellar concentration of SDS in the mobile phase on the PVA column was compared to the retention behavior on other types of columns.