• Journal of the Korean Chemical Society
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• v.43 no.1
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• pp.7-119
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• 1999

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.4 no.2
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• pp.189-197
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• 1994

Analytic methods for Cr(VI) level in industrial hygienic field were suggested by the National Institute for Occupational Safety and Health(NIOSH method 7600, 7604). There were growing needs for measurement of Cr(III) and Cr(VI) levels simultaneously. Two analytical methods were suggested to determine Cr(III) and Cr(VI) levels simultaneously. The one is method by using reversed phase high peformance liquid chromatography(HPLC) and the other is by using ion exchange HPLC. The purpose of this work was to evaluate the usefulness of these two analytic methods. For the difference of ionic charges of Cr(III)-ethylendiamine tetraacetic acid(EDTA) chelate and $CrO_4{^-2}$, we could detect them simultaneously by ion exchange HPLC. Also, we attempted to determine the levels of Cr(III) and Cr(VI) chelated with sodium diethyldithiocarbamate(NaDDTC) by using reversed phase HPLC. The confirmation of Cr(III) and Cr(VI) were checked by fraction collector and nameless atomic absorption spectrometer. The optimal conditions for the formation of Cr(III)-EDTA chelate were two hours incubation period with pH 5. Cr(III)-EDTA and Cr(VI) in EDTA solution were successfully separated by anion exchange column using $Na_2CO_3/NaOH$ mixture as mobile phase. Peaks of Cr(III)-EDTA and Cr(VI) in EDTA were identified at 5 minutes and 7 minutes of retention time respectively by the ion exchange HPLC. The formation of Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates were twelve hours incubation period. Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates were separated by reversed phase column using methanol and water mixture as mobile phase. Peaks of Cr(VI)NaDDTC and Cr(III)-NaDDTC chelates were identified at 13 minutes and 26 minutes of retention time respectively by the reversed phase HPLC. Due to reduction of Cr(VI) to Cr(III), it seems to be not suitable for simultaneous determination of Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates by reversed phase HPLS. Simultaneos determination of Cr(III) and Cr(VI) by ion exchange HPLC was more accurate and simple method.

• Archives of Pharmacal Research
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• v.23 no.6
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• pp.568-573
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• 2000

A reversed-phase high-performance liquid chromatographic method was developed to determine the optical purity of bevantolol enantiomers. (S)-(-)-Menthyl chloroformate((-)-MCF), (S)-(-)-$\alpha$-methylbenzyl isocyanate((-)-MBIC) and 2,3,4,6-tetra-O-acetyl-$\beta$-D-glucopyranosyl isothiocyanate(GITC), which can react with the secondary amine group of bevantolol were investigated as chiral derivatization reagents. Among them indirect chiral HPLC method using CITC gave the best result. The derivatization proceeded quantitatively within 20 min at room temperature. Separation of the enantiomers as diastereomers was achieved by reversed-phase HPLC within 20min using ODS column. Different ratios of (S)-(-)-bevantolol and (R)-(+)-bevantolol were prepared. Enantiomeric separation of these mixtures took place on a chiralcel OD column or, after derivatization with GITC, on a ODS column. No racemization was found during the experiment. This method allowed determination of 0.05% of either enantiomer in the presence of its stereoisomer and method validation showed adequete linearity over the required range.

• Bulletin of the Korean Chemical Society
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• v.14 no.4
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• pp.510-514
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• 1993

The retention behavior of proteins was investigated by using reversed-phase chromatography (RPC), comparing to the retention behavior of small molecules in RPC. The evaluation was carried out on a SynChropak RP-P($C_{18}$) column with 0.1% aq. TFA-organic solvent modifier such as acetonitrile, isopropanol, and ethanol. The Z value (the number of solvent molecules required to displace the solute from the surface) was a general index for the characterization of protein retention as a function of organic concentration over a range of temperature between 5 and 70$^{\circ}C$. Van't Hoff plots provided the basis for evaluating the enthalpic and entropic changes associated with the interaction between protein and the stationary phase. Z values did not change significantly at the range of temperature showing the consistent ${\Delta}H^{\circ}$ and ${\Delta}S^{\circ}$ values. From these investigation, it was concluded that the retention behavior of proteins in RPC was able to be predicted by the retention parameters applied to small molecules. Furthermore, myoglobin and hemoglobin in RPC as stated above showed a similar retention behavior regardless of their molecular weights.

• Journal of the Korean Chemical Society
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• v.39 no.4
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• pp.257-265
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• 1995

Free amino acids were isolated from milk and their absolute amounts were determined by reversed phase high performance liquid chromatography after derivatization with dansyl chloride. The determination of D- and L-amino acids was based on achiral separation on a C18 column. It was found that milk contained totally 41.00 mg DL-amino acids in 100 mL milk. The level of D-amino acids to L-amino acids was determined by a column-switching system combining an achiral reversed phase separation and chiral chelate additive. The chiral separation was carried out with addition of the chiral Cu(N-benzyl-L-proline)2 chelate to the mobile phase in reversed phase liquid chromatography. It was found that the determination of 16 different amino acids is feasible in the milk sample with a C18 column separation and 12 D-amino acids out of the 16 amino acids can be determined via the column-switching system with chiral separation. 2.05% of D-glutamic acid and 2.93% of D-alanine were found in milk.

• Journal of the Korean Chemical Society
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• v.36 no.6
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• pp.849-856
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• 1992

We prepared a simple, economic and versatile preparative system for an enantiomeric separation. Hydrophobic amino acid enantiomers were resolved in the preparative scale by a centrifugal liquid chromatography on the N-hexadecyl-L-proline coated reversed phase. The factors controlling the retention and resolution of racemic amino acids such as the concentration of Cu(Ⅱ), pH of the eluent, the type and content of organic modifier, and rpm of CLC were examined. Several mg of hydrophobic amino acid enantiomers were separated preparatively. To separate all of different amino acid enantiomers, various coating material will be investigated.

• 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.

• Mass Spectrometry Letters
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• v.9 no.3
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• pp.77-80
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• 2018

The focus of this paper is to present techniques to overcome certain difficulties in quantitative analysis with a time-of-flight mass spectrometer (TOF-MS). The method is based on conventional solid-phase extraction, followed by reversed-phase ultra high performance liquid chromatography of the extract, and mass spectrometric analysis. The target compounds included atenolol, atrazine, caffeine, carbamazepine, diclofenac, estrone, ibuprofen, naproxen, simazine, sucralose, sulfamethoxazole, and triclosan. The matrix effects caused by high concentrations of organic compounds in wastewater are especially significant in electrospray ionization mass spectroscopy. Internal-standard calibration with isotopically labeled standards corrects the results for many matrix effects, but some peculiarities were observed. The problems encountered in quantitation of carbamazepine and triclosan, due to nonlinear calibration were solved by changing the internal standard and using a narrower mass window. With simazine, the use of a quadratic calibration curve was the best solution.

• Korean Journal of Pharmacognosy
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• v.21 no.3
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• pp.239-241
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• 1990

A new method for quantitative determination of byakangelicin in Angelicae dahuricae Radix by high performance liquid chromatography was established. A reversed-phase system with a ${\mu}Bondapak$ $C_{18}$ column using THF : dioxane : MeOH : HAc : 5% $H_3PO_4$ : $H_2O$=72.5 : 62.5 : 25 : 10 : 1 : 329 as a mobile phase was developed. Byakangelicin together with ter-O-byakangelicin and oxypeucedanin methanolate, and isooxypeucedanin as an internal reference were detected at 350 nm and the analysis was successfully carried out within 30 min.

• Korean Journal of Pharmacognosy
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• v.30 no.3
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• pp.328-331
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• 1999

A new method for quantitative determination of p-methoxycinnamic acid in Scrophulariae radix by high performance liquid chromatography was established. A reversed-phase system with SPHERI-5 RP-18 5 micron $(250\;{\times}\;4.6\;mm)$ column using TFA (0.05%) and acetonitrile as a mobile phase was developed. p-Methoxycinnamic acid and N-(p-methoxycinnamoyl)-p-aminophenol as an internal reference were detected at 310 nm and the analysis was successfully carried out within 50 min.