• Bulletin of the Korean Chemical Society
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• v.27 no.1
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• pp.71-76
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• 2006

Porous polymer monolithic columns were prepared by the direct free radical copolymerization of methacrylic acid and ethylene glycol dimethacrylate within the confines of a chromatographic column in the presence of toluene-dodecanol as a porogenic solvent. The separation characteristics of the monolithic columns were tested by a homologous series of xanthine derivatives, theophylline and caffeine. The effects of the polymerization mixture composition and polymerization condition, mobile phase composition, flow rate and temperature on the retention times and separation efficiencies were investigated. The results showed that the selection of correct porogenic solvents and appropriate polymerization conditions are crucial for the preparation of the monolithic stationary phases. The separation efficiency was only extremely weakly dependent on flow rate and temperatures. Hydrogen-bonding interaction played an important role in the retention and separation. Compared with conventional particle columns, the monolithic column exhibited good stability, ease of regeneration, high separation efficiency and fast analysis.

• Journal of the Korean Chemical Society
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• v.53 no.2
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• pp.137-143
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• 2009

Liquid chromatographic enantiomer separation of N-tert-butoxycarbonyl (BOC) $\alpha$-amino acids and their ethyl esters was performed on covalently immobilized chiral column (Chiralpak IC) derived from polysaccharide derivative. The solvent versatility of the covalently immobilized Chiralpak IC in enantiomer separation of N-BOC $\alpha$-amino acid ethyl ester derivatives was shown and the chromatographic parameters of their enantioselectivities and resolution factors were greatly influenced by the nature of the mobile phase. Also the effect on the dissolving solvent for these analytes on the enantiomer separation using the same mobile phase and the examples of preparative enantiomer separation on analytical column were shown.

• Bulletin of the Korean Chemical Society
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• v.31 no.8
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• pp.2322-2328
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• 2010

A multiple solid-phase extraction (SPE) method was used with liquid chromatography, coupled with mass spectrometry (LC/MS), for the analysis of heterocyclic amines (HCAs) in human urine. Separation efficiencies based on the pH of the mobile phase and the types of columns were compared. An amide column showed better baseline separation and narrower HCA peak widths at pH 5.0 for the mobile phase than a $C_8$ column. Each SPE step, HLB, MCX, and HybridSPE, was optimized by controlling the pH conditions. The combined method with the three SPEs effectively removed interfering species that cause ion-suppression during HCA detection. Validation of the method, performed with SIM and SRM detection, showed correlation coefficients above 0.991 in the range 0.3 - 16.7 ng/mL. Recovery rates were 45.4 - 97.3% on the $C_8$ column and 71.8 - 101.4% on the amide column, and method detection limits were 0.11 - 0.65 ng/mL on the $C_8$ column and 0.12 - 0.48 ng/mL on the amide column. This method using multiple SPEs offers significant benefits for high-throughput determination of HCAs in urine.

• Analytical Science and Technology
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• v.37 no.2
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• pp.123-129
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• 2024

We present a rapid method for the determination of Cs, Sr, and Ba, heat generators found in highly active liquid wastes, by gas-pressurized extraction chromatography (GPEC) using a column containing a cation-exchange resin. GPEC is a microscale column chromatographic technique that uses a constant flow rate of solvent (0.07 mL/min) with pressurized nitrogen gas supplied through a valve. In particular, because this method uses a small sample volume (a few hundred microliters), it produces less chemical waste and allows for faster separation compared to traditional column chromatography. In this study, we evaluated the separation of Cs, Sr, and Ba using GPEC. The eluate from the column (GPEC or conventional column chromatography) was quantitatively analyzed using inductively coupled plasma-mass spectrometry to measure the column recovery and precision. The column reproducibility of the proposed GPEC system (RSDs of recoveries) ranged from 2.7 to 4.1 %, and the column recoveries for the three elements ranged from 72 to 98% when aqueous HCl was used as the eluent. The GPEC results are slightly different in efficiency and separation resolution compared to those of conventional column chromatography because of the differences in the eluent flow rate as well as the internal diameter and length of the column. However, the two methods had similar recoveries for Cs and Sr, and the precision of GPEC was improved by two-fold. Remarkably, the solvent volume required for GPEC analysis was five times lower than that of the conventional method, and the total analysis time was 11 times shorter.

• Archives of Pharmacal Research
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• v.23 no.5
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• pp.441-445
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• 2000

Achiral-chiral column switching HPLC assay was developed to allow the separation and quantification of the enantiomers of terbutaline in human plasma by means of fluorescence detection. Plasma samples were prepared by solid-phase extraction with sep-pak silica, followed by HPLC assay. The enantiomers of terbutaline and the internal standard were separated from the biological matrix on a silica column, and the two enantiomers were resolved and quantified on a Sumichiral OA-4900 column. The two columns were connected by a switching valve equipped with silica trap column, The trap column was used to concentrate the terbutaline in the eluent from the achiral column before back flushing onto the chiral phase. For each enantiomers, the assay was linear between 2.5-125 ng/$m\ell$ (r=0.9999) and detection limit was 1.0 ng/$m\ell$ .

• 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.

• Proceedings of the PSK Conference
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• 2002.10a
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• pp.398.2-398.2
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• 2002

A column switching HPLC assay was developed to allow the separation and quantitation of cetirizine in human plasma by ultraviolet (UV) detection. Plasma samples were prepared by liquid-liquid extraction. After drying, the residue was reconstituted in 20 mM phosphate buffer (pH 2.8) containing 15% acetonitrile. The samples were initially injected onto a clean-up Capcell Pak MF C18 column. (50 mm $\times$ 4.6 mm I.D.), and the chromatographic region containing the peaks of interest was followed in an analytical C18 microcolumn (250 mm$\times$1.5 mm I. D.) via column switching device. (omitted)

• Archives of Pharmacal Research
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• v.21 no.2
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• pp.212-216
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• 1998

A coupled achiral-chiral high-performance liquid chromatographic system has been developed for the determination of the enantiomers of salmeterol, S-(+)-salmeterol and R-(-)-salmeterol in urine. THe salmeterol was separated from the interfering components in urine and quantified on the silica column, and the enantiomeric composition was determined on a Sumichiral OA-4700 chiral stationary phase. The two columns were connected by a switching valve equipped with a silica precolumn. The two columns wer connected by a switching valve equipped with a silica precolumn. The precolumn was used to concentrate the salmeterol in the eluent from the achiral column before backflushing onto the chiral phase. The coupled system was validated.

• Korean Journal of Pharmacognosy
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• v.16 no.3
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• pp.175-179
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• 1985

The optimal condition for the determination of saikosaponin a and d, the major pharmacologically active saponins of the roots of Bupleurum falcatum, was studied with the conversion of these saponins into diene saponins $(saikosaponin\;b_1\;and\;b_2)$. The complete separation and quantitative analysis of these saponins were performed by the method of high performance liquid chromatography using $NH_2$ column. The conversion of saikosaponin a and d into diene saponins under gastric pH was calculated. Thirty-three percent of saikosaponin a was converted to saikosaponin $b_1$ and 63 percent of saikosaponin d was converted to saikosaponin $b_2$.

• Bulletin of the Korean Chemical Society
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• v.25 no.9
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• pp.1336-1340
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• 2004

The same kind of chiral stationary phase with a commercialized chiral column was used to make preparative chiral columns and was applied to resolve racemic N-acetyl-1-naphthylethylamide (3) by preparative liquid chromatography. An improved chromatographic condition to resolve racemic 3 on the CSP was examined by changing flow rate and kind of the mobile phase and the sample injection volume. The optimized separation conditions were applied to resolve racemic 1,1'-Binaphthyl-2,2'-diamine(4).