• Bulletin of the Korean Chemical Society
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• v.19 no.6
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• pp.619-624
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• 1998

A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBS) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

• Journal of Microbiology and Biotechnology
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• v.5 no.5
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• pp.302-304
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• 1995

As the previous HPLC method (Ogasawara et al., 1983) was described for the analysis of aclacinomycin A and some of its analogue compounds but not for aclacinomycin Y, we developed novel HPLC condition by optimizing solvent system. The newly developed solvent system allowed a complete separation of aclacinomycins Y and A, as opposed to the incomplete resolution of these two compounds in conventional method. The amounts of aclacinomycins Y and A could be accurately determined when the fermentation broth of Streptomyces lavendofoliae DKRS was analyzed by the newly developed method.

• Analytical Science and Technology
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• v.16 no.1
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• pp.78-81
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• 2003

Peptides separation in high performance liquid chromatography (HPLC) is very important for the analysis of total proteins using mass spectrometry rather than two-dimensional polyacrylamide gel electrophoresis (2D-PAGE). In this study, we investigated the optimal HPLC condition of peptides for the use of mass fingerprinting. As a result of pursuing a combination of solvent additives for HPLC, water and acetonitile containing both 0.1% trifluoroacetic acid and 0.1% acetic acid respectively showed the most efficient resolution and sensitivity.

• KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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• v.1 no.1
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• pp.20-28
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• 1995

The conditions of Soxhlet extraction and HPLC analysis were examined for the determination of antioxidants used for polyolefins manufacturing. The extraction with methylene chloride in a Soxhlet apparatus for 10 hours and above provides almost complete recovery of the additives from polyolefins. The determination of the antioxidants including BHT, Irganox 1076, Irganox 1010 and Irgafos 168 could be successfully performed by using reversed-phase HPLC under gradient elution where the baseline separation of all four antioxidants in a single run was possible. In addition, the antioxidants inherently contained in commercial LLDPE and OPP films were identified and quantitatively determined.

• Food Science of Animal Resources
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• v.21 no.1
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• pp.64-70
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• 2001

The extraction procedure and HPLC condition were modified to analyze the residues of oxytetracycline, sulfamethoxazole and chloramphenicol in pork, simultaneously. The antibacterial agents in pork were extracted with 0.02M EDTA-Mcilivine buffer:ethanol:acetonitrile (5:3:2). After the removal of fat with n-hexane, the extracts were evaporated and purified with Sep-pak $C_{18}$ cartridge column using 0.01M oxalic acid 0.1% (v/v) triethylamine (TEA) in acetonitrile. The peak of antibacterial agents was detected with $\mu$ Bondapak C18 column, UV detector (280nm) and 0.01M oxalic acid: methanol: acetonitrile (7.5:2.0:0.5). Detection limits for three antibacterial standards were 0.03 ppm. Calibration curves were linear between 0.03 and 2.0 ppm (R$^2$>0.999). When spiked the level of 1.0 ppm of oxytetracycline, sulfamethoxazole and chloramphenicol into meats, the recoveries from meats were 77.3%, 79.7% and 59.3%, respectively. These results showed that the modified extraction method provided good analytical resolution and the recoveries of the above antibacterial agents in meats.

• Analytical Science and Technology
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• v.36 no.4
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• pp.143-151
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• 2023

Considering the greater role of α-amino acids in our daily lives, the enantiomer resolution of seven α-amino acids derivatized with fluorogenic reagent (4-fluoro-7-nitro-2,1,3-benzoxadiazole, NBD-F) by chiral HPLC on amylose or cellulose trisphenylcarbamate derived chiral stationary phases (CSPs) under simultaneous ultraviolet (UV) and fluorescence (FL) detection was performed. The degree of enantioseparation and resolution was affected by nature and selector backbones of the CSPs as well as the kind of amino acids. Baseline enantiomer separation and resolutions were observed for the enantiomers of all analytes as NBD derivatives especially on coated type amylose tris(3,5-dimethylphenylcarbamate) derived CSPs (Chiralpak AD-H and Lux Amylose-1). The other CSPs also showed good enantioselectivity except for the CSPs (Chiralpak IB, Chiralcel OD-H and Lux Cellulose-1) having cellulose tris(3,5-dimethylphenylcarbamate) as chiral selectors. The developed analytical chiral method was applied to determine the enantiomeric purity of seven commercially available L-α-amino acids and the impurities as D-forms were found to be in the range 0.08-0.87 %, respectively. The intra- and interday accuracy and precision assays showed high accuracy and precision of the developed analytical method. This chiral HPLC method for the enantiomer resolution of amino acids using fluorescent derivatization could be useful for the determination of enantiomeric purity of pharmaceuticals and biological study for amino acid type compounds among chiral drugs.

• Korean Chemical Engineering Research
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• v.48 no.1
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• pp.88-92
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• 2010

DNA structure studies attract many interests in pharmaceutical, biochemical and medical disciplines. Among them, base pairs play a vital role in biological information transfer. Therefore, they need to be analyzed in various ways and the pair of guaninine and cytosine is the present analytical object. Separation of guanine and cytosine was researched by Aspen chromatography simulator and HPLC(High Performance Liquid Chromatography) experiments. Aspen chromatography simulation resulted in various chromatograms with changes of sample concentration, eluent flow rate and number of plate. The resolutions and yields of guanine and cytosine were calculated to obtain a best separation condition. $C_{18}$ HPLC column and water/methanol/acetic acid mixture(90/10/0.2) were used for separation of guanine and cytosine. HPLC parameters(resolution and number of theoretical plate) were calculated under different flow rates and sample concentrations. Aspen chromatography simulation and HPLC experimental results were compared with fair agreement.

• KSBB Journal
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• v.20 no.3
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• pp.244-249
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• 2005

Chiral separation of racemic ibuprofen was achieved on a Kromasil KR100-5CHI-TBB column. Some chromatographic parameters (resolution, number of theoretical plates, HETP, capacity factor) are calculated under different separation conditions such as change of mobile phase compositions (hexane / t-BME : 85 / 15, 75 / 15, 65 / 35, 55 /45) as well as acetic acid concentrations for adjusting pH (0.1 to 1 $v/v\%$). Flow rate versus number of theoretical plates and HETP were compared to evaluate column efficiency. To determine the adsorption isotherms, PIM (Pulsed Input Method) was carried out. At concentrations of racemic ibuprofen between 0.1 and 0.3 mg/ml, S- and R-ibuprofen have the same retention time of 4.48 and 5.81 min. Ibuprofen isotherms show a linear form under concentrations of 0.3 mg/ml with eluent (hexane / t-BME = 55 / 45).

• Bulletin of the Korean Chemical Society
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• v.23 no.9
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• pp.1291-1294
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• 2002

Various racemic N-protected ${\alpha}-amino$ acids such as N-t-BOC-(tert-butoxycarbonyl), N-CBZ-(benzyloxycarbonyl) and N-FMOC-(9-fluorenylmethyloxycarbonyl) ${\alpha}-amino$ acids were resolved as their anilide and 3,5-dimethylanilde derivatives on an HPLC chira l stationary phase (CSP) developed by modifying a commercial (S)-leucine CSP. The chromatographic resolution results were compared to those on the commercial (S)-leucine CSP. The resolutions were greater on the modified CSP than those on the commercial CSP with only one exception, the resolution of N-t-BOC-phenylglycine anilide. In addition, the chromatographic resolution behaviors were quite consistent except for the resolution of N-protected phenylglycine derivatives, the (S)-enantiomers being retained longer. Based on the chromatographic resolution behaviors and with the aid of CPK molecular model studies, we proposed a chiral recognition mechanism for the resolution of N-protected ${\alpha}-amino$ acid derivatives. However, for the resolution of N-protected phenylglycine derivatives, a second chiral recognition mechanism, which competes in the opposite sense with the first chiral recognition mechanism, was proposed. The two competing chiral recognition mechanisms were successfully used in the rationalization of the chromatographic behaviors for the resolution of N-protected phenylglycine derivatives.

• YAKHAK HOEJI
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• v.50 no.1
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• pp.21-25
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• 2006

Reiterated normal-phase column chromatography lead to the isolation and purification of six known compounds but for the first time from the whole plant of Sasa borealis (Hack.) Makino (Gramineae): tricin 4'-O-(erythro-${\beta}$-guaia-cylglyceryl) ether (1), tricin 4'-O-(threo-${\beta}$-guaiacylglyceryl) ether (2), tricin 4'-O-[erythro-${\beta}$-guaiacyl-(9'-O-acetyl)-glyceryl] ether (3), tricin 4'-O-[threo-${\beta}$-guaiacyl-(9'-O-acetyl)-glyceryl] ether (4), (-)-pinoresinol (5), and vanillin (6). The structures of the compounds (1-6) were established based on interpretation of high resolution NMR (COSY, HSQC, HMBC, and NOESY) spectral data. In particular, compounds 1 and 3 were diastereomers of compounds 2 and 4, respectively. These two sets of diastereomers were able to be simultaneously identified and quantified by a gradient reversed-phase HPLC method with UV photodiode array, This sensitive HPLC method is noteworthy as a simultaneous separation and identification method to test the extract of the family Gramineae which contains these compounds.