• Mass Spectrometry Letters
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• 제5권1호
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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.

• 한국미생물·생명공학회지
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• 제20권3호
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• pp.335-343
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• 1992

미생물이 생산하는 대사길항물질을 screening한 결과 최소검정배지에서 Gram 양성균에 항균활성을 나타내고 L-leucine에 의하여 그 항균활성이 길항당하는 182-27 물질을 생산하는 방선균을 토양에서 새로이 분리하였다. 본 생산균을 분류 동정한 결과, 유연균을 찾아볼 수가 없고 신 균종으로 동정하기에는 많은 type culture와의 비교분류를 하여야만 하므로 여기서는 다만 기균사의 포자형성과 세포벽 성분의 조성, 형태학적 성상 등으로 보다 Streptomyces sp.로만 동정하였다. 182-27 균주의 배양조건을 검토하고 최적조건에서 대량 배양하여 그 배양여액으로부터 이온교환수지, silica gel column chromatography 등에 의하여 활성 물질을 분리 정제하였으며 배양액 약 20$\ell$에서 약 20mg의 백색분말을 얻었다. 182-27 물질은 그의 이화학적 성질로 보아 아미노산 유연물질로 추정할 수가 있으나 그의 화학구조는 아직 밝히지 못했다. 생물학적 성질은 최소검정배지상에서 Gram 양성균에 항균력을 나타냈고 이러한 항균력은 L-leucine의 첨가에 의해 저해 당했다.

• 한국진공학회지
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• 제19권1호
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• pp.36-44
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• 2010

관경이 수 mm인 세관 램프 내부에서 플라즈마의 확산을 조사하기 위하여 이극성(ambipolar) 확산방정식을 해하였다. 반경 방향의 확산에 의한 유리관 벽에서의 플라즈마 소멸 특성시간은 $\tau_r\;=\;(r_0/2.4)^2/D_a$로 주어진다. 반경 $r_0{\sim}1\;mm$이고 이극성 확산계수 $D_a{\sim}0.01\;m^2/s$ 이면, $\tau_r{\sim}17\;{\mu}s$이다. 이는 램프의 교류전원 구동에서 플라즈마를 유지하기 위한 구동 최소 주파수 ~30 kHz에 해당한다. 고전압이 인가되는 전극부에 발생한 고밀도의 플라즈마가 양광주로 확산되는 특성시간은 $\tau_z{\sim}0.1\;s$이다. 고밀도 플라즈마 경계에서의 시간에 대한 확산속도는 $t{\sim}10^{-6}\;s$일 때 $u_D{\sim}10^2\;m/s$이고, $t{\sim}10^{-3}\;s$이면 그 속도는 $u_D{\sim}1\;m/s$로 느려진다. 따라서 램프 길이 ~1 m에 대하여 전극부에서 생성된 고밀도 플라즈마가 양광주 전체로 확산되는 시간은 수 초가 걸린다.

• Mass Spectrometry Letters
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• 제8권4호
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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.

• 대한수의학회지
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• 제33권1호
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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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• 제10권4호
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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.

• 한국전산구조공학회:학술대회논문집
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• 한국전산구조공학회 2006년도 정기 학술대회 논문집
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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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• 제15권4호
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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.

• 한국환경농학회지
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• 제29권3호
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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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• 제11권5호
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• pp.536-542
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• 1996

충치 예방 물질의 탐색 연구 일환으로, Cacao bean husk(CBH) 추출물로부터 얻어진, gluco-syltransferase(Gtase) 저해 활성 분획을 분리하였 다. 이를 다시 MCI-gel CHP-20와 Sephadex LH 20의 column chromatography법으로 분리, 정제하였으며, 이로부터 얻어진 2개의 GTase 활성 저해 물질에 대한 구조 해석을 행하였다. 분리.정제된 2개의 GTase 저해 활성 물질은 anisaldehyde-$H_2SO_4$ 및 FeCb에서 각각 갈색 및 청색 반응을 하며, 또 TLC상에서 dimer의 flavan-3-ol $R_r$값을 나타내는 단일 물질이었다. NMR(PMR, C CMR) 빛 mass spectrum으로 두 정제 분획에 대 한 화학 구조를 분석한 결과, G Tase 저해능을 나타 내는 단물질은 (-)-epicatechin-($\beta\rightarrow8$)-catechin 으로 결합된 procyanidin B-1 ($C_{30}H_{26}O_{12}$) 및 cate chin의 2량체인 procyanidin B一3($C_{30}H_{26}O_{12}$)이었다.