• Bulletin of the Korean Chemical Society
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• v.22 no.4
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• pp.409-412
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• 2001

Poly(p-tert-butyltrimethoxymonopropyloxycalix[4]arene-methylsiloxane) (TBCX-MS) has been prepared and used as a stationary phase in isothermal capillary gas chromatographic separation of some positional isomers. Retention factors (k) and separatio n factors $(\alpha)$ for the isomers were measured and compared with those on poly(p-tert-butyl-dimethoxydipropyloxycalix[4]arene-tetramethyldisiloxane) (TBCX-TMDS), poly(dimethoxydipropyloxycalix[4]arenetetramethyl-disiloxane) (CX-TMDS). Most of the isomers investigated are well resolved on TBCX-MS. Retention of all the compounds decreases on the three phases in the order, TBCX-TMDS ${\geq}$ TBCX-MS > CX-TMDS. Similar retention values on TBCX-TMDS and TBCX-MS seem to indicate that retention property of the two phases is not significantly affected by the spatial position of the calixarene moiety.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.27 no.2
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• pp.123-129
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• 2017

Objectives: The purpose of this study is to enhance the application of analytical method of polar solvents(alcohols) by GCOTC (gas chromatography open tubular column) through the system suitability test(SST) to estimate the whole chromatographic system performance(integral part). Methods: To perform the SST, carried out repeatability(n=6) as analytical method of polar solvents by GCOTC, got the retention time($t_R$), standard deviation(${\sigma}_{n-1}$) of $t_R$, baseline width($w_b=4{\sigma}_{n-1}$) and calculated dead time($t_m$) by $v_m=d^2{\pi}L(f/4)$ and $v_m=t_m$ x flow rate. Results: In this experiment, obtained the basic data, there were $t_m=2$ min, methanol($t_R=3.569$, ${\sigma}_{n-1}=0.01$, $w_b=0.04$), ethanol ($t_R=3.892$, ${\sigma}_{n-1}=0.004$, $w_b=0.016$), isopropanol($t_R=4.209$, ${\sigma}_{n-1}=0.004$, $w_b=0.016$). By using these data, calculated the corrected retention time($t_R{^{\prime}}$), capacity factor(k), separation factor(${\alpha}$), number of theoretical plate(n) and resolution($R_s$) for SST and got the good results. Conclusions: Through the SST, could reconfirm the whole chromatographic performance system(integral part) for analytical method of polar solvents by GCOTC. Therefore, this analytical method expect to be widely applied at the related areas.

• KSBB Journal
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• v.11 no.5
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• pp.529-535
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• 1996

Methyl frucloside was purified from the aqueous sugar/methyl fructoside solution by liquid chromatography using Amberlite IRA-900, strong anion-exchange resin. The optimum operating conditions, resolution and productivity of methyl fructoside were discussed to evaluate the practical feasibility of the proposed chromatographic separation process of methyl fructoside which is useful as a new starting material for sugar ester synthesis. The linear chromatography model with HETP was well applied to the chromatographic separation process of methyl fructoside and the theoretical solution successfully predicted the elution chromatogram of methyl fructoside and sucrose at different superficial linear velocity of eluent for rectangular feed with different loading volume of packed bed. The optimum operating conditions were found to be 75% with the loading volume of packed bed at 1.13 cm/min of the superficial linear velocity at $60^{\circ}C$, and gave the productivity of methyl fructoside of 7 mg/g-resin/h with the resolution of 1.1.

• Analytical Science and Technology
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• v.23 no.4
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• pp.405-413
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• 2010

A new method for the simultaneous determination of six glucocorticoids (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, and flumethasone) in meats (bovine muscle, bovine liver) were established. Samples were effectively extracted using C18 cartridge with ethylacetate. Chromatographic separation was achieved using C18 column and negative electrospray ionization mass spectrometry was performed in the Multiple Reaction Monitoring mode for the effective quantitation and qualification of glucocorticoids. Acetonitrile and water (0.1% formic acid) were used as mobile phase and additive for effective electrospray ionization, and gave good chromatographic separation and mass spectrometric sensitivity. The limit of detection (LODs) and the limit of quantitation (LOQs) in spiked blank samples depending on types of matrix and pharmaceuticals were ranged from 0.2 to $1.0\;{\mu}g$/kg and 0.8 to $3.4\;{\mu}g$/kg, respectively. And the recoveries were between 89.5 to 119.6%. The established method showed good recoveries, accuracies, precisions and fast sample preparation and it will be applied to assay of glucocorticoids residues in meat.

• 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.

• Analytical Science and Technology
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• v.36 no.1
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• pp.32-43
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• 2023

This study reports for the first time about a stability indicating RP-HPLC method for qualitative and quantitative determination of acalabrutinib in bulk and dosage form and in presence its impurities 1, 2 and 3. The chromatographic separation was carried on Zorbax XDB-C18 (250×4.6 mm; 5 µ id) as stationary phase, Phosphate buffer pH 6.4 and methanol 80:20 (v/v) as mobile phase at a flow rate of 1.0 mL/min, UV detection was carried at wavelength of 238 nm and the analysis was completed with a run time of 15 min. In these conditions the retention time of acalabrutinib and its impurities 1, 2 and 3 was observed to be 3.50, 4.83, 8.40 and 9.93 min respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50 %, 100 % and 150 % was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for acalabrutinib and both impurities studied and the % RSD in each spiked level was found to be less than 2. Stability tests were done through exposure of the analyte solution to five different stress conditions i.e expose to 1N hydrochloric acid, 1 N sodium hydroxide, 3 % peroxide, 80 ℃ temperature and UV radiation at 254 nm. In all the degradation condition, standard drug acalabrutinib was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis there is no other chromatographic detection of other impurities and formulation excipients. Hence the developed method was found to be suitable for the quantification of acalabrutinib and can separate and analyse impurities 1 and 2.

• 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.

• KSBB Journal
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• v.26 no.4
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• pp.323-327
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• 2011

The convenient derivatization method of chiral amino alcohols as 9-anthraldimine Schiff base derivatives for chiral resolution was developed and the liquid chromatographic enantiomer separation of chiral amino alcohols as 9-anthraldimine derivatives was investigated on several coated and covalently bonded polysaccharide-derived chiral stationary phases (CSPs). In general, the performance of Chiralcel OD-H (or Chiralcel OD) (${\alpha}$ = 1.24-2.89), the coated CSP derived from cellulose derivative was superior to the other CSPs for resolution of 9-anthraldimine derivatives of several amino alcohols. The results of enantioseparation depending on the structure of 9-anthraldimine analytes like the steric bulky group and the polar moiety etc were discussed. The analytical method was applied to measure the enantiomeric purity of commercially available chiral amino alcohols. It is expected that the convenient analytical method will be very efficient for determination of enantiomeric purity of amino alcohols as 9-anthraldimine Schiff base derivatives with strong UV absorption.

• Korean Journal of Pharmacognosy
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• v.15 no.3
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• pp.139-146
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• 1984

High performance liquid chromatographic separation is described for the analysis of bile acids after hydrolysis in seven commercial crude bile drugs and ox and pig galls. They are simultaneously separated with HPLC mobile phase of acetonitrile/0.5% ammonium carbonate (pH 6.7) (25.5 : 74.5) at a flow rate $(1.0{\rightarrow}1.5ml/min.)$ and differential refractometer. The linearity of calibration curve and recovery test are good by using the method. The analysis of major bile acids in seven commercial crude bile drugs using the described method is presented. Sample no. 1 of them is similar to separation pattern of ox gall. Sample no. 6 of them is supposed to be genuine bear gall on the basis of identification of ursodeoxycholic acid. Sample $no.\;2{\sim}5$ and 7 of them are supposed to be pig gall on the basis of identification of hyodeoxycholic acid which is a characteristic component of pig gall.

• Bulletin of the Korean Chemical Society
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• v.35 no.7
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• pp.2033-2037
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• 2014

A reaction mixture was developed for formation of soft organic monolith that was easily smashed, rinsed, refluxed, filtered, and dried to give monolith particles having high pore volume of macropores. This phase was almost without mesopores. The reaction mixture was composed of methacrylic acid, ethylene glycol dimethacrylate, polyethylene glycol (porogen), and an initiator in a mixed solvent of toluene and isooctane. The selection of porogen and its amount was carefully carried out to obtain the optimized separation efficiency of the resultant phase. The median macropore size was 1.6 ${\mu}m$, and the total pore volume was 3.0-3.4 mL/g. The median particle size (volume based) was 15 ${\mu}m$, and the range of particle size distribution was very broad. Nevertheless the column (1 ${\times}$ 300 mm) packed with this phase showed good separation efficiency (N~10,000-16,000) comparable to that of a commercial column packed with 5 ${\mu}m$ C18 silica particles.