• Bulletin of the Korean Chemical Society
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• 제24권9호
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• pp.1265-1268
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• 2003

The estimation of retention factors by correlation equations with physico-chmical properties maybe helpful in chromatographic work. The physico-chemical properties were water solubility (S), hydrophobicity (P), total energy ($E_t$), connectivity index 1 ($^1{\chi}$), hydrophilic-lipophlic balance (x) and hydrophilic surface area (h) of isoflavones. The retention factors were experimentally measured by RP-HPLC. Especially, the empirical regulations of water solubility and hydrophobicity were expressed in a linear form. The equation between retention factors and various physico-chemical properties of isoflavones was suggested as $k = a_0 + a_1\;log S + a_2log\;P^Q + a_3(E_t) + a_4(^1{\chi}) + a_5(x) + a_6(h)$, and the correlation coefficients estimated were relatively higher than 0.95. The empirical equations might be successfully used for a prediction of the various chromatographic characteristics of substances, with a similar chemical structure.

• 분석과학
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• 제22권4호
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• pp.313-318
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• 2009

다당유도체를 기초로 하는 키랄 컬럼들을 사용하여 여러 amino alcohol의 거울상 이성질체를 산 또는 염기 등의 첨가제가 포함된 이동상에서 액체크로마토그래피로 광학분리를 수행하였다. 산 또는 염기 등의 첨가제가 각각 포함된 이동상뿐만 아니라 사용한 키랄 컬럼에 따라 광학분리된 선택성과 분리 인자가 크게 영향을 받았다. 특히 Chiralcel OD 컬럼에서 이동상에 0.1% trifluoroacetic acid를 산 첨가제로 사용했을 경우 0.1% triethylamine을 염기 첨가제로 사용했을 경우보다 머무름인자 값은 더 작게 나타났지만 광학분리의 선택성과 분리인자는 크게 증가됨을 보여주었다. 또한 Chiralcel OD 컬럼에서 이동상에 0.05% trifluoroacetic acid와 0.05% triethylamine을 함께 사용했을 때 광학분리의 선택성과 분리인자가 어느 이동상 조건보다도 가장 좋은 광학분할 결과를 보여주었다.

• 약학회지
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• 제37권1호
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• pp.1-8
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• 1993

A procedure for the high-performance liquid chromatographic determination of Nebramycin factors in fermentation broth of Streptoalloteichus hindustanus ATCC 31218 mutant was investigated using pre-column derivatization and LTV detection. The method is based on pre-column derivatization of Nebramycin factors with 2,4-dinitrofluorobenzene(DNFB) in the presence of Tris (hydroxymethyl)aminoethane. The chromatographic separation of derivatives of Nebramycin factors and unknown impurities is achieved using reversed-phase column (NOVA-PAK $C_{18}$, Waters Co.) and AcCN : H$_{2}$O : AcOH (53.0:46.5:0.5) as a mobile phase. The mixture of these derivatives were separated within 35 minutes and the optimum wavelength($\lambda_{max}$ ) of the UV detector was 353 nm. The linearity of response for derivatives of Nebramycin factors is demonstrated for concentrations up to 500 $\mu\textrm{g}$/ml and the relative standard deviation is less than 0.79%. Detection limit was 1.67 ng for the 10 $\mu\textrm{l}$ sample volume employed.

• Bulletin of the Korean Chemical Society
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• 제27권2호
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• pp.211-218
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• 2006

This work deals with 24 substances composed of nitrogen-containing heterocycles. The relationships between the chromatographic retention factor (k) and those physicochemical properties which are relevant in quantitative structure-properties relationship (QSPR) studies, such as the polarizability $(\alpha)$, molar refractivity (MR), lipophilicity (logP), dipole moment $(\mu)$, total energy $(E_{tot})$, heat of formation $(\Delta H_f)$, molecular surface area $(S_M)$, and binding energy $(E_b)$, were investigated. The accuracy of the simple linear regressions between the chromatographic retention and the descriptors for all of the compounds was satisfactory (correlation coefficient, $0.8 \leq r \leq 1.0$). The QSPR models of these nitrogen-containing heterocyclic compounds could be predicted with a multiple linear regression equation having the statistical index, r = 1.000. This work demonstrated the successful application of the multiple linear approaches through the development of accurate predictive equations for retention factors in liquid chromatography.

• 대한화학회지
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• 제55권5호
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• pp.751-755
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• 2011

A doubly tethered chiral stationary phase (CSP) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid was applied to the resolution of various aryl ${\alpha}$-aminoalkyl ketones with the use of 80% ethanol in water containing 10 mM sulfuric acid as a mobile phase. The chiral resolution was quite successful, the separation factors (${\alpha}$) and the resolutions ($R_S$) being in the range of 1.39-2.05 and 3.18-5.22, respectively. The separation factors (${\alpha}$) on the doubly tethered CSP were slightly worse than those on the corresponding singly tethered CSP. However, the resolutions ($R_S$) on the doubly tethered CSP were generally greater than those on the corresponding singly tethered CSP. The chromatographic behaviors for the resolution of aryl ${\alpha}$-aminoalkyl ketones on the doubly tethered CSP were demonstrated to be dependent on the type and the content of the organic and acidic modifiers in aqueous mobile phase and the column temperature.

• KSBB Journal
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• 제29권3호
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• pp.205-209
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• 2014

Chromatographic enantiomer resolution of chiral amines was performed on several covalently immobilized and coated chiral stationary phases (CSPs) based on polysaccharide derivatives under the mobile phase conditions containing base or acid or acid/base additive. The chromatographic parameters including separation factors and capacity factors were greatly influenced by the nature of the mobile phase containing base or acid or salt additive as well as the used CSPs. When 0.05% triethylamine/0.05% trifluoroacetic acid as an additive in the mobile phase was used on all CSPs in this study, the greatest enantiomer resolution was observed except for Chiralpak AD. Also, it was shown that the change of base additive into acid or salt in the mobile phase may directly affect chiral recognition mechanisms between the chiral selectors and analytes occurring during enantiomer separation, resulting in the change of elution orders.

• Bulletin of the Korean Chemical Society
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• 제24권12호
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• pp.1757-1762
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• 2003

The interrelation between retention factors of several L-amino acids and their physico-chemical and structural properties can be determined in chromatographic research. In this paper we describe a predictor for retention factors with various properties of the L-amino acids. Eighteen L-amino acids are included in this study, and retention factors are measured experimentally by RP-HPLC. Binding energy ($E_b$), hydrophobicity (log P), molecular refractivity (MR), polarizability (${\alpha}$), total energy ($E_t$), water solubility (log S), connectivity index (${\chi}$) of different orders and Wiener index (w) are theoretically calculated. Relationships between these properties and retention factors are established, and their predictive and interpretive ability are evaluated. The equation of the relationship between retention factors and various descriptors of L-amino acids is suggested as linear and multiple linear form, and the correlation coefficients estimated are relatively higher than 0.90.

• Bulletin of the Korean Chemical Society
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• 제28권11호
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• pp.1980-1984
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• 2007

An HPLC chiral stationary phase (CSP) which has only two ureide functional groups was prepared starting from (1S,2S)-1,2-diaminocyclohexane. The CSP was successful in the resolution of various N-(3,5- dinitrobenzoyl)-α-amino acids, the separation (α) and the resolution factors (RS) being within the range of 1.11-1.35 and 2.19-5.17, respectively with the use of 20% 2-propanol in hexane containing 0.1% trifluoroacetic acid as a mobile phase. However, ethyl esters of N-(3,5-dinitrobenzoyl)-α-amino acids were not resolved or resolved with only marginal separation and resolution factors on the CSP under the identical mobile phase condition. From these results, the complexation of the carboxylate anions of analytes inside the double-ureide pocket of the CSP was expected to play some important role for the chiral recognition. In contrast, N-(3,5- dinitrobenzoyl)-α-amino acid N-propylamides were resolved on the CSP with reasonable separation and resolution factors. Enantioselective hydrogen bonding interactions between analytes and the CSP were presumed to be responsible for these resolutions.

• Mass Spectrometry Letters
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• 제12권1호
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• pp.1-10
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• 2021

A simple, specific, and economical LC-MS/MS method was investigated for the screening of 43 prescribed antihypertensive and related drugs in human urine. The urine samples were simply prepared by diluting and mixing with internal standard before directly introduced to the LC-MS/MS system, which is fast, straightforward, and cost-effective. Fractional factorial, Box-Behnken, and I-optimal design were applied to screen and optimize the mass spectrometric and chromatographic factors. The analysis was carried out on a triple quadrupole mass spectrometer system utilizing multiple reaction monitoring with positive and negative electrospray ionization method. Chromatographic separation was performed on a Thermo Scientific Accucore RP-MS column (50 × 3.0 mm ID., 2.6 ㎛) using two separate gradient elution programs established with the same mobile phases. Chromatographic separation was performed within 12 min. The optimal method was validated based on FDA guideline. The results indicated that the assay was specific, reproducible, and sensitive with the limit of detection from 0.1 to 50.0 ㎍/L. The method was linear for all analytes with coefficient of determination ranging from 0.9870 to 0.9981. The intra-assay precision was from 1.44 to 19.87% and the inter-assay precision was between 2.69 and 18.54% with the recovery rate ranges from 84.54 to 119.78% for all drugs measured. All analytes in urine samples were stable for 24 h at 25℃, and for 2 weeks at -60℃. The developed method improves on currently existing methods by including larger number of cardiovascular medications and better sensitivity of 12 analytes.

• Bulletin of the Korean Chemical Society
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• 제29권5호
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• pp.979-984
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• 2008

In this study, 8 solutes (aniline, caffeine, p-cresol, ethyl benzene, methylparaben, phenol, pyridine, and toluene) have been tested in terms of linear solvation energy relationships (LSER). Several micellar liquid chromatography (MLC) systems using cationic surfactant cetyltrimethylammonium bromide (CTAB) and a mixture of water with (methanol, n-propanol, and n-butanol) modifiers were characterized using the LSER solvation parameter model. The effects of the surfactant and modifier concentration on the retention in MLC were discussed. LSER model had demonstrated high potential to predict retention factors with high squared correlation coefficients ($r^2$ > 0.99). A comparison of predicted and experimental retention factors suggests that LSER formalism is able to reproduce adequately the experimental retention factors of the solutes studied in the different experimental conditions investigated. This model is a helpful tool to understand the solute-surfactant interactions and evaluate the retention characteristic of micellar liquid chromatography.