• Mass Spectrometry Letters
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• v.5 no.1
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• pp.24-29
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• 2014

An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

• Microbiology and Biotechnology Letters
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• v.20 no.3
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• pp.335-343
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• 1992

A Streptomyces strain No. 182-27, which produced amino acid antimetabolite, was isolated from soil. During the course of screening for new amino acid antimetabolites from the culture broths of Actinomycetes, we found that the strain produced a substance active against Gram-positive bacteria and its activity was reversed by L-Ieucine on the synthetic minimal agar medium in the culture broth. The morphological and cultural characteristics serve to identify the producing organism strain 182-27 as the Streptomyces, although the species of this strain should be resolved in further studies. Fermentation was carried out in the synthetic medium at $28^{\circ}C$ for 78 hours. The fermentation yield reached about 2 mg per liter of the broth. Purification was done by ion exchange resin, active carbon, silica gel column chromatography and obtained 20 mg of pure active substance from the 20 $\ell$ culture broth. The 182-27 substance was obtained as white powder, mp 18SoC. From the physicochemical characteristics of the substance, it was amino acid like substance but unknown about its chemical structure. It is active against some Gram-positive bacteria and reversed by L-Ieucine.

• Journal of the Korean Vacuum Society
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• v.19 no.1
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• pp.36-44
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• 2010

The ambipolar diffusion equation has been solved in a fine-tube lamp of a few mm in diameter. In the diffusion of radial direction, the plasma diffuses and vanishes away at the glass wall by recombination with the characteristic time of plasma loss is given by $\tau_r\;=\;(r_0/2.4)^2/D_a$. With the radius $r_0{\sim}1\;mm$ and the ambipolar diffusion coefficient $D_a{\sim}0.01\;m^2/s$, the vanishing time is calculated $\tau_r{\sim}10\;{\mu}s$ which corresponds to the least value of frequency 30 kHz for the sustaining the plasma in the operation of high voltage AC-power. In the diffusion of longitudinal z-direction, a high density plasma generated at the area of a high voltage electrode, diffuses into the positive column with the characteristic time $\tau_z{\sim}0.1\;s$. The plasma diffusion velocity at the boundary of high density plasma is $u_D{\sim}10^2\;m/s$ at the time $t{\sim}10^{-6}$ s and the diffusion velocity becomes slow as $u_D{\sim}1\;m/s$ at $t{\sim}10^{-3}\;s$. Therefore, for the long lamp of 1 m, it takes about several seconds for the high density plasma at the area of electrode to diffuse through the whole positive column space.

• Mass Spectrometry Letters
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• v.8 no.4
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• pp.90-97
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• 2017

Androgenic anabolic steroids (AASs) are synthetic derivatives of testosterone with a common structure containing cyclopentanoperhydrophenanthrene nucleus. Their use enhances the muscle building capacity and is beneficial during performance. The AASs are one of the most abused group of substances in horse doping. Liquid chromatography tandem mass spectrometry ($LC/MS^n$) has been successfully applied to the detection of anabolic steroids in biological samples. However, the saturated hydroxysteroids viz: nandrolone, $5{\alpha}-estrane-3{\beta}$, $17{\alpha}-diol$ exhibit lower detection responses in electrospray ionisation (ESI) because of their poor ionisation efficiency. To overcome this limitation pre-column chemical derivatization has been introduced to enhance their detection responses in $LC-ESI-MS^n$ analysis. The aim of present study was to develop a sensitive method for identification and confirmation of nandrolone and its metabolite in horse urine incorporating pre-column derivatization using picolinic acid. The method consists of extraction of targeted steroid conjugates by solid phase extraction (SPE). The eluted steroid conjugates were hydrolysed by methanolysis and free steroids were recovered with liquid-liquid extraction. The resulting steroids were derivatized to form picolinoyl esters and identification was done using LC-ESI-MS/MS in positive ionization mode. The picolinated steroid adduct enhanced the detection levels in comparison to underivatized steroids.

• Korean Journal of Veterinary Research
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• v.33 no.1
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• pp.61-69
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• 1993

In order to search for new antibiotics from anaerobic bacteria, a large number of samples from domestic soil were collected and processed by apropriate methods. A potential strain, Streptococcus sp. An-21-1, was found to produce antimicrobial compounds. The Results were as follows; 1. During fermentation, the bacteria grew rapidly up to 20hr, thereafter entered the death phase. The optimal temperature and pH for the bacterial growth were $37^{\circ}C$ and pH 7.0, respectively. 2. Antibiotics were purified from culture broth by solvent extraction, silica gel column chromatography and Sepadex L.H 20 column. 3. Physicochemical properties of Ap-1 and Ap-2 were similar ; Their melting points were between $234-237^{\circ}C$. Color reactions of ninhydrin, 2,7-dichlorofluorescein, 4-dimethylaminobenzaldehyde, Dragendroffs reagent and 20% $H_2SO_4$, were positive. Therefore, we assumed that these antibiotics have amine group, immine group, alkaloid, and lipid components. These were stable to heat. UV spectrophotometry showed two peaks at 210 nm and 260 nm. From above results, we assumed these antibiotics are belong to the peptide antibiotic family.

• Advances in concrete construction
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• v.10 no.4
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• pp.319-332
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• 2020

The impacts of reinforcing concrete matrix with steel fibers, polypropylene fibers and recycled plastic fibers using different volume fractions of 0.15%, 0.5%, 1.5% and 2.5% on the compressive and tensile characteristics are experimentally investigated in the current research. Also, flexural behavior of plain concrete (PC) beams, shear performance of reinforced concrete (RC) beams and compressive characteristics of both PC and RC columns reinforced with recycled plastic fibers were studied. The experimental results showed that the steel fibers improved the splitting tensile strength of concrete higher than both the polypropylene fibers and recycled plastic fibers. The end-hooked steel fibers had a positive effect on the compressive strength of concrete while, the polypropylene fibers, the recycled plastic fibers and the rounded steel fibers had a negative impact. Compressive strength of end-hooked steel fiber specimen with volume fraction of 2.5% exhibited the highest value among all tested samples of 32.48 MPa, 21.83% higher than the control specimen. The ultimate load, stiffness, ductility and failure patterns of PC and RC beams in addition to PC and RC columns strengthened with recycled plastic fibers enhanced remarkably compared to non-strengthened elements. The maximum ultimate load and stiffness of RC column reinforced with recycled plastic fibers with 1.5% volume fraction improved by 21 and 15%, respectively compared to non-reinforced RC column.

• Proceedings of the Computational Structural Engineering Institute Conference
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• 2006.04a
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• pp.421-426
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• 2006

To examine the behaviors of traditional wooden structural frame in Korea in direction of beam, an experimental study was performed. The interior frame of Daewoongjeon of Bongjeongsa was selected as a model, which has two short exterior columns and one high inside column. The experimental frame has 1/2 scale and lateral forces are applied at high inside column by using drift control. The vertical gravity loads are applied on the frame. From the results of experiment it was shown that the stiffness and lateral capacity of the frame was increased when vertical loads are applied and the force-drift relationship in positive load direction was not same as in negative load direction. And push-over analysis are performed by using macro model in which the rotational and shear springs which were derived from the another experiments of subassemblies were used. The numerical analysis with macro model showed a good correspondence with the experiment within 2% story drift.

• Archives of Pharmacal Research
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• v.15 no.4
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• pp.347-355
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• 1992

To elucidate structure of group "a" epitope, mouse antibodies that express idiotype monoclonal antibody and anti-idiotype monoclonal antibody against the group specific "a" determinant were purified by hydroxyapatite column. To obtain hepatitis B surface antigens (HBsAg). HBsAg positive blood was sequencially purified by ammonium sulfate precipitation, hydroxyapatite, sepharose 4B column chromatography and ultracentrifugation. The major protein (p25) and glycoprotein (gp30) of HBsAg were isolated by concanavalin-A-sepharose 4B. The ability of p25-gp30 among the HBsAg to inhibit the idiotype-anti-idiotype reaction was dependent on conformation, since reduced and alkylated p25-gp30 virtualy lost their inhibitory capacity when compared to native HBsAg. The data suggest that hepatitis B antigen is a conformational antigen critically dependent upon the disulfide bonds of p25-gp30.

• Korean Journal of Environmental Agriculture
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• v.29 no.3
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• pp.247-256
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• 2010

A high-performance liquid chromatographic (HPLC) method was developed to determine buprofezin residues in hulled rice and fruits. The buprofezin residue was extracted with acetone and the extract was stepwise purified by liquid-liquid partition and Florisil column chromatography. For rice samples, acetonitrile/n-hexane partition was additionally employed to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate buprofezin from sample co-extractives, as detected by ultraviolet absorption at 250 nm. Recovery experiment at the limit of quantitation validated that the proposed method could evidently determine the buprofezin residue at the level of 0.02 mg/kg. Mean recoveries from hulled rice, apple, pear, and persimmon samples fortified at three tenfold levels were in the range of 80.8~85.2%, 89.1~98.4%, 88.8~95.7% and 90.8~96.2%, respectively. Relative standard deviations of the analytical method were all less than 5%, irrespective of sample types. A selected-ion monitoring LC/mass spectrometry with positive electrospray ionization was also provided to sensitively confirm the suspected residue.

• KSBB Journal
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• v.11 no.5
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• pp.536-542
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• 1996

The isolation of active compounds showing the inhibitory effect on glucosyltransferase(GTase) from cacao bean husk(CBH) extract was carried out for screening of anti-plaque agents. These active compounds were purified by additional column chromatography of MCI-gel CHP-20 and Sephadex LH-20 and their chemical structures were determined by NMR and mass spectroscopy. Two compounds showing the inhibitory effect on GTase from CBH extract were obtained. These compounds showed positive reactions with anisaldehyde-H2SO4 solution and FeCl3, and were identified as dimeric flavan-3-ols on TLC. By NMR and MS data analyses, the structures of two different flavan-3-ols were identified as procyanidin B-1 and procyanidin B-3, respectively.