• Analytical Science and Technology
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• v.5 no.1
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• pp.63-71
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• 1992

Liquid chromatographic behavior of Pd(II), Ni(II) and Co(III) in N-Alkylisonitrosoacetylacetone imine(HIAA-NR) chelates was investigated by reversed phase high perfomance liquid chromatography. The optimum conditions for the separation of IAA-NR-metal chelates were examined respect to the flow rate and mobile phase strength. The metal-N-Alkylisonitrosoacetylacetone imine chelates in solution were successfully separated on Novapak $C_{18}$ column using acetonitrile/water mixture as mobile phase. The elution order of chelates is methyl>ethyl>propyl>butyl as N-alkyl group for ligand is varied. It was found that all IAA-NR-metal chelates were eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of log k' on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extraction distribution ratio(Dc) in acetonitrile-water-alkane extraction system was investigated for IAA-NR-metal chelate. Both kinds of dependence are linear, which suggests that the retention of the electroneutral metal chelates on Novapak $C_{18}$ column is largely due to the hydrophobic effect.

• Analytical Science and Technology
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• v.12 no.1
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• pp.28-33
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• 1999

Glutathione(GSH) in biological samples was determined by high performance liquid chromatographic(HPLC) method with fluorescence detector(FLD) after monobromobimane(MBB) or 4-fluoro-7-sulfobenzofurazan(SBD-F) derivatization. The detection limit of $0.03{\mu}g/mL$ was obtained after MBB derivatization, derivative of MBB was about 200 times more sensitive than that of SBD-F. N-acetylcysteine was used as internal standard and tetrabutylammonium ion as counter ion for better separation. The determination by ion-pairing chromatography after MBB derivatization was characterized by linearity in the range between $0.08{\sim}8.33{\mu}g/mL$ with a good correlation coefficient of 0.998. By precision test appeared relative standard deviation at less than 5% at three different concentrations. This method can be used for the analysis of GSH in plasma and tissue.

• Journal of the Korean Chemical Society
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• v.31 no.3
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• pp.236-243
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• 1987

The optimum resolution condition of 11 organophosphorus pesticides by gas-liquid chromatography was studied using a capillary column. The injection modes and types of vaporization tubes were evaluated in relation to pesticide analysis. The best reproducibility of peak heights of pesticides was obtained by the split mode with the vaporization tube packed with quartz wool. A 25m SE-30 capillary column provided better resolution than SE-54 column for their optimum resolution. The column at $200^{\circ}C$ initially was heated by $5^{\circ}C/min\;to\;230^{\circ}C$ followed by $10^{\circ}C/min\;to\;270^{\circ}C$ and the temperatures were held constant for 5 minutes at $230^{\circ}C\;and\;270^{\circ}C$, respectively. The relative standard deviations of their retention times were less than 0.19%.

• Journal of the Korean Chemical Society
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• v.35 no.6
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• pp.720-724
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• 1991

Simultaneous determination of chloragenic acid (CA), 3,4-o-dicafeoyl quinic acid(3,4-DCQA), 4,5-o-dicaffeoyl quinic acid (4,5-DCQA) and linarin in Chrysanthemum sibiricum Fisher was newly established by a reversed-phase high performance liquid chromatography (HPLC). Sample was extracted with 20 ml methanol for 4 hrs. The extract was cleaned up by using Sep-Pak $C_18$ cartridge and 4 ml methanol-$H_2$O(1 : 1) as eluent. Their determination was performed by means of RP-HPLC with Bondapak $C_18$ column (30 cm ${\times}$ 3.9 mm i.d., 10 ${\mu}m$ and gradient elution mode as methanol-5 mM $H_3PO_4$ solution (30 : 70). The established method was applied to various samples purchased. As a result, their content ranges showed to be 0.35~0.55% for CA, 0.46~0.76% for 3,5-DCQA, 0.077~0.23% for 4,5-DCQA and 0.16~2.72% for linarin, respectively.

• KSBB Journal
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• v.23 no.2
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• pp.135-141
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• 2008

SMB (simulated moving bed) chromatography is a very useful utility for the separation of binary system. We simulated the separation of L-arabinose and L-ribose from the mixture by using lab-scale 4(1-1-1-1)-zone SMB chromatography. Preliminary experiments of PIM (pulse input method) were performed to measure adsorption isotherms of L-ribose and L-arabinose in $NH_2$ HPLC column, and experimental and simulated results from ASPEN chromatography were compared. To find the most suitable separation condition in SMB, we carried out a simulation in $m_2-m_3$ plane base on the triangle theory and calculated operating parameters (flow rate of four zone, switching time and feed concentration and so on) using ASPEN chromatography under the conditions of linear isotherms obtained from PIM.

• Korean Chemical Engineering Research
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• v.43 no.6
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• pp.715-721
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• 2005

The SMB chromatography is used to obtain high purification of fructooligosaccharides (FOS), the mixture of kestose and nystose. SMB operation condition is usually determined by triangle theory or standing wave design when reactions do not occur within columns during experiment. Some of the reactions in columns may considerably affect experimental results. FOS can be hydrolyzed and converted into glucose and fructose during operation. To include the effect of reaction, the concentrations of each component at steady state after hydrolysis were used in simulation. The obtained simulation values are well matched with experimental results except sucrose. For sucrose, the experimental results were different from expected one due to the existence of an intermediate component. FOS is easily hydrolyzed and converted into glucose and fructose in more acidic condition and at higher temperature. Hydrolysis reaction can be prevented by the pretreatment of separation resin with NaOH as well as operation under lower temperature.

• Microbiology and Biotechnology Letters
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• v.15 no.6
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• pp.375-380
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• 1987

D-$\alpha$-Amino-$\varepsilon$-carpolactam racemase (EC 5.1.1) and L-$\alpha$-amino-$\varepsilon$-caprolactam hydrolase (EC 3.5.2) were fractionated from cell-free extracts of Alcaligenes eutrophus A52 using ammonium sulfate precipitation and DEAE-cellulose ion exchange chromatography. It was made sure that D-$\alpha$-amino-$\varepsilon$-caprolactam was converted to L-$\alpha$-amino-$\varepsilon$-caprolactam by racemase, and then hydrolyzed into L-lysine by hydrolase in Alcaligenes eutrophus A52. For the conversion of D-$\alpha$-amino-$\varepsilon$-caprolactam into L-lysine by cell-free extracts of Alcaligenes eutrophus A52, the optimum temperature and pH were 6$0^{\circ}C$ and 8.5 respectively. The results showed that 0.5% D-$\alpha$-amino-$\varepsilon$-caprolactam was converted to L-lysine at 55$^{\circ}C$ for 10 hr with a conversion rate of 98% by cell-free extracts containing 3.1mg of protein.

• Applied Chemistry for Engineering
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• v.8 no.2
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• pp.315-319
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• 1997

In this study, the optimum analytical conditions for determination of distribution of propylene oxide in a nonionic surfactant and separation of fatty alcohols were investigated by Reversed Phase High Performance Liquid Chromatography. To analyse the distribution of propylene oxide (PO) and carbon chain length of a fatty alcohol, we derivatized samples for the purpose of using a UV detector. Also, we studied the influences of columns and mobile phase composition to obtain the optimum separation conditions. In our experiment, Waters Symmetry $C_8(3.9{\times}150mm)$ column was used. And the optimum condition were obtained by gradient elution with methanol and water as the mobile phase. In the plot of log k' vs composition of water in the binary phase, the linerality was very good. We ploted the calibration curve to conform the quality of fatty alcohol, a good linerality was obtained.

• Applied Chemistry for Engineering
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• v.8 no.2
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• pp.286-291
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• 1997

Taxol which is recognized as a powerful anticancer reagent was extracted from yew extract and separated by NP-HPLC (Normal-PhaseHigh Performance Liquid Chromatography). The experiments were performed in the isocratic mode with $5{\mu}l$ to $100{\mu}l$ injection volume and 1ml/min mobile phase flow rate. The major mobile phase was hexane and small amounts of ethanol, methanol, 1-propanol and isopropanol were added to change the retention behavior. Prior to a real sample, the artificial mixture of taxol, cephalomannine and 10-deacetyltaxol was tested. They are hard to be separated because of similar chemical structures. The experimental results showed that the proper composition of mobile phase for separating the three components was found 96% hexane and 4% ethanol(vol.%) or 96% hexane, 2% 1-propanol and 2% methanol(vol.%). Compared to the run time of 80 minutes for the binary system, the mixture was separated within 50 minutes with the less amount of mobile phase for the ternary system. Finally, $1{\mu}g$ of taxol was separated from yew tree extracts under the optimum operating conditions.

• Analytical Science and Technology
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• v.8 no.3
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• pp.259-264
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• 1995

The separation efficiency of metal ions by using the poly-NTOE(1, 12-diaza-3, 4:9, 10-dibenzo-5, 8-dioxacyclopentadeca-1, 12-ylene-2, 7-dihydroxyoctamethylene) has been determined by column chromatography in aqueous solution. Binding constants and separation factors for several poly-NTOE interactions were measured in aqueous solution. The order of these binding constants and separation factors with metal ions were Co(II)Zn(II) for the transition metal ions and Cd(II)