• Title/Summary/Keyword: column method

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Determination of volatile and residual iodine during the dissolution of spent nuclear fuel (사용 후 핵연료 용해 중 휘발 및 잔류 요오드 분석)

  • Kim, Jung Suk;Park, Soon Dal;Jeon, Young Shin;Ha, Young Keong;Song, Kyuseok
    • Analytical Science and Technology
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    • v.22 no.5
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    • pp.395-406
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    • 2009
  • The determination of iodine in the spent nuclear fuel and the volatile behavior during its acid dissolution have been studied by NAA(neutron activation analysis) and electron probe microanalysis (EPMA). Simulated spent fuels (SIMFUELs) were dissolved in $HNO_3$(1+1) at $90^{\circ}C$ for 8 hours. The iodine remained in a dissolver solution after dissolution, and that condensed in dissolution apparatus and trapped in the adsorbent by volatilization during the dissolution were determined, respectively. The condensed iodine was recovered by the redistillation with $HNO_3$(1+1) after transfer of the dissolver solution. The iodines in the dissolver and redistilled solution were separated by solvent extraction followed by ion exchange or precipitation method and determined by RNAA (radiochemical neutron activation analysis). The ion exchange column and filtration kit used for the isolation of iodine, which were prepared with a polyethylene tube, were used as an insert in the pneumatic tube for neutron irradiation. The iodine volatilized during the dissolution of SIMFUELs was collected in a trapping tube containing Ag-silica gel (Ag-impregnated silica gel) adsorbent, and the distribution of iodine trapped in the adsorbents were determined by EPMA. The adsorbing characteristics shown with the SIMFUELs were compared with those shown with a real spent fuel from the nuclear power plant.

Analysis of clenbuterol in bovine muscle and milk by LC-ESI/MS/MS (LC-ESI/MS/MS를 이용한 소고기와 우유에서의 클렌부테롤 분석)

  • Hong, Selyung;Jeong, Jiyoon;Park, Hyejin;Lee, Soonho;Lee, Jongok
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.535-542
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    • 2008
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

Structural Performance Evaluation of Anchors for Power Equipment Electrical Cabinets Considering On-Site Installation Conditions (현장 설치 조건을 고려한 발전설비 전기 캐비닛 정착부 앵커의 구조성능 평가)

  • Lee, Sang-Moon;Jung, Woo-Young
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.43 no.6
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    • pp.709-719
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    • 2023
  • In general, most of the electrical equipment responsible for control within power plants is housed in self-standing cabinets. These cabinets are typically fixed to a slab using post-installed anchors. Although the fixation method of using post-installed anchors provides stability, there is a risk of conductor failure due to external forces, including moments. However, the performance assessment of current anchors is only evaluated through uniaxial material tests. Therefore, the primary purpose of this study is to compare the static performance of post-installed anchors, considering on-site installation conditions, with their performance in material tests and to analyze the behavioral characteristics of the anchors. While conducting experiments using actual cabinets would be ideal, practical and spatial constraints make this approach difficult. As an alternative, experiments were conducted using a test specimen consisting of a steel column and a support. As a result, the pull-out performance of anchors reflecting on-site installation conditions was measured to be about 10% higher than that observed in material tests. The trends in load reduction and the point of maximum performance for the anchors also differed. To verify the reliability of the experimental study, a 3D FEM analysis was performed, which will provide predictive information on the loads transferred to the post-installed anchors for structural performance evaluations of electrical cabinets using shaking table test in the future.

Development of Simultaneous Analytical Method of Veterinary Antibiotics in Manure using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS를 이용한 퇴비 및 액비 중 항생제 동시 분석법 개발)

  • Chung, Hyung Suk;Lee, Young Jun;Lee, Han Sol;Rahman, Md. Musfiqur;Kabir, Md. Humayun;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.201-210
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    • 2017
  • BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

Determination of methamphetamine, 4-hydroxymethamphetamine, amphetamine and 4-hydroxyamphetamine in urine using dilute-and-shoot liquid chromatography-tandem mass spectrometry (시료 희석 주입 LC-MS/MS를 이용한 소변 중 메스암페타민, 4-하이드록시메스암페타민, 암페타민 및 4-하이드록시암페타민 동시 분석)

  • Heo, Bo-Reum;Kwon, NamHee;Kim, Jin Young
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.161-170
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    • 2018
  • The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

Simultaneous Determination and Monitoring of Three Macrolide Antibiotics in Foods by HPLC (Macrolide계 항생물질 동시분석법 확립 및 모니터링)

  • Park, Sang-Ouk;Lee, Sang-Ho;Ahn, Jong-Hoon;Jung, Young-Ji;Kim, Seong-Cheol;Kim, Ji-Yeon;Keum, Eun-Hee;Sung, Ju-Hyun;Kim, Sang-Yub;Jang, Young-Mi;Kang, Chan-Soon
    • Korean Journal of Food Science and Technology
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    • v.42 no.3
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    • pp.287-291
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    • 2010
  • In this study, a simple and rapid pre-treatment method based on liquid extraction was applied for the simultaneous determination of three macrolides (spiramycin, tylosin, and tilmicosin) residues. In these studies, the stock farm products was used as a matrix sample. When the liquid extraction method was compared with the solid phase extraction (SPE) method, the former showed higher recovery percentages and simpler steps than the latter. The macrolids were separated using a reverse-phase C18 ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$) column and a gradient elution with mobile phases consisting of phosphate buffer (pH 2.5) and acetonitrile. Tylosin and tilmicosin were detected at 288 nm and spiramycin was detected at 232 nm. The average recovery percentage ranged between 83.0-90.2% for samples spiked with the three macrolids at 50 and 100 ng/g The validation results showed that the limit of detection (7 (spiramycin), 12 (tilmiconsin), 12 (tylosin) ng/g)) was under the regulatory tolerances and the linearity from calibration curves was satisfactory for determining the multi-residue of three macrolids in farm products. Monitoring samples were collected at the main cities in Korea as Seoul, Busan, Deajeon, Incheon, Deagu, and Gwangju. Microlide antibiotics were not detected in most samples.

Determination of several families of antibacterial agent residues in fish by disk assay (미생물학적 방법에 의한 어체내 잔류 항균물질의 계열별 동정시험)

  • Jung, Sung-Hee;Kim, Jin-Woo
    • Journal of fish pathology
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    • v.10 no.2
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    • pp.125-135
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    • 1997
  • The possibility of identification of families of antibacterial agent residues in fish tissue was studied by disk assay using three test organisms, Bacillus subtilis BGA, Micrococcus luteus ATCC 9341, and Bacillus cereus var. mycoides ATCC 11778. In the present method, a simple clean-up procedure was performed to obtain the aqueous solution from homogenized flounder muscle sample(10g) in Mcilvaine buffer. Then, aqueous solution was fractionated into A and B to be used in disk assay by choloroform and Sep-Pak $C_{18}$ cartridge column after being defatted in hexane. The chloroform layer of fraction A was used for the analysis of macrolide antibiotics(ML), sulfa drugs(SA), chloramphenicol(CP), and quinolone antibiotics(QN). Adsorbed materials to Sep-Pak $C_{18}$ of fraction B were also employed for the analysis of penicillins(PC), tetracyclines(TC), and nitrofuran derivatives(NF) Minimun-detectable concentrations by the present method were, $0.1{\mu}g$/g for oxytetracycline, tetracycline, doxycycline, spiramycin and ciprofloxacin, $0.025{\mu}g$/g for erythromycin and ampicillin, $1.0{\mu}g$/g for sodium nifurstyrenate and florfenical, $0.25{\mu}g$/g for sulfamonomethoxie and sulfadimethoxine, $2.5{\mu}g$/g for oxolinic acid and flumequine, and $15{\mu}g$/g for piromidic acid, respectively. Three test organisms showed different sensitivity patterns for each family of antibacterial agent. Sensitivity patterns were B. cereus > B. subtilis > M. luteus for TC and NF, M. luteus > B, subtilis > B. cereus for ML and PC, B. cereus = B. subtilis > M. luteus for CP and QN, and B. subtilis > B. cereus=M. luteus for SA. The present method utilizing these characteristics could be useful as a routine screening test for the determination of family of antibacterial agent residues in fish tissue.

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Study on the Planning Method of the Sacheonwangsa Temple Architecture in Silla (신라사천왕사건축(新羅四天王寺建築)의 설계기술(設計技術) 고찰(考察))

  • Lee, Jeongmin;Mizoguchi, Akinori
    • Korean Journal of Heritage: History & Science
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    • v.53 no.3
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    • pp.80-109
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    • 2020
  • The Sacheonwangsa Temple in Silla is an esoteric temple that was founded provisionally in 670, and was completed in 679. This study attempted to elucidate the planning method of the Sacheonwangsa Temple based on the results of research on excavations and investigations into its construction processes and construction measures thereof. The research results are as follows. (1) In the site construction, assuming the size of one Bang (坊) on the south of Nangsan Mountain, after dividing the north-south width into three equal parts, there is a possibility that two of these parts were set to the flat portion. (2) In the 'Jochang (祖創, 670)', it is estimated that an area of 300 cheoks by 300 cheoks was postulated on the flat surface, and, as an initial conception, the mandala's plane design of the outer square 2 hasta (3 cheoks) and inner square 1 hasta (1.5 cheoks) was originally devised for the setting of 'Mudra (神印)', and an area 100 times greater has been set as the basis in the scale and layout planning of the central block. (3) During 'Gaechang (攺刱, ~679)', it is judged that because of the narrowness of the distance between the Pagoda and Geumdang Hall, which occurs when the center of the Geumdang Hall coincides with the center of 'the first stage of the foundation (先築基壇)', the scale and layout planning were adjusted from the initial conception. (4) The arrangement of the building was determined by dividing the fixed size of the central block (280 cheoks by 320 cheoks). Specifically, the east-west direction is set on the quartile's line of the east-west width of the central block, and in contrast, the north-south direction is based on the structural characteristics of the central block. It is presumed that the position of the transept was determined through the division and adjustment of the column spacing of the east-west corridor, then the Geumdang Hall and Altar were based on this. (5) The scale of the Geumdang Hall and Pagoda is determined by the petition of the division by the unit fraction starting from the quartile's line of the central block's east-west width. This planning is understood to be based on the self-similarity, which is rooted in the mandala's plane design as the model.

Antioxidant Activities of Stachys sieboldii MIQ Roots (초석잠(Stachys sieboldii MIQ) 뿌리 추출물의 항산화 활성 고찰)

  • 백홍석;나영수;김도한;이창한;류병호;송승구
    • Journal of Life Science
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    • v.14 no.1
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    • pp.1-7
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    • 2004
  • The root of Stnchys Sieboldif MIQ was extracted three times with methanol and extract was found to contain 3.02% of polyphenols and 1.97% of flavonoids. DPPH radical scavenging method, ferric thiocyanate method, and nitrite scavenging ability method were employed to investigate the constituents of the extract and to measure their activity on antioxidation. The fraction extracted by ethylacetate showed higher anti oxidation value than that of $\alpha-tocopherol$, butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) at the same concentration. UV-VIS spectral data of the extract by ethylacetate that was isolated on a silica gel column proved adsorption maxima in the range of 280∼330 nm. The fraction ES-RS that has $\lambda_{max}(nm)$ of band 1, 325nm and band II, 289nm exhibitd the strongest activity on antioxidation. ES-R5 fraction showed similar pattern to flavones by the analysis of UV-VIS spectral data.

$^{99m}Tc$ Labeling Kit Preparation and Characteristics of Anti-NCA-95 Monoclonal Antibody (항 NCA-95 단일클론항체의 $^{99m}Tc$표지 키트 제조 및 특성 연구)

  • Hong, Mee-Kyoung;Jeong, Jae-Min;Chung, June-Key;Choi, Seok-Rye;Kim, Chae-Kyun;Lee, Yong-Jin;Lee, Dong-Soo;Lee, Myung-Chul;Koh, Chang-Soon
    • The Korean Journal of Nuclear Medicine
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    • v.30 no.4
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    • pp.541-547
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    • 1996
  • The previous monoclonal antibody labeling method for bone marrow immunoscintigrapy was complicated and laborious for clinical application. Also it showed a relatively low labeling efficiency. To improve this procedure, we compared several direct labeling methods of $^{99m}Tc$. 1) The labeling efficiency in the method using gluconate as a transchelator was low (40-70%), but immunoscintigraphy using this radiotracer produced a clear image. 2) To improve labeling efficiency, ${\beta}$-mercaptoethanol was removed after reduction. The labeling efficiency was improved up to 70-80%, but the radioactivity of the blood pool was high. 3) The higest labeling efficiency (>90%) and best quality images could be obtained by using MDP as a transchelating agent. It did not require additional procedures for separation of labeled antibodies. The immunoreactivity of this antibody was 60%. Residual MDP which can be taken up by the bone could be removed by PD-10 column. The reduced antibodies were stable with a high labeling efficiency (>90%) for up to 47 days by deep freezing. We concluded that the improved procedure for $^{99m}Tc$ labeling of anti-NCA-95 monoclonal antibody using MDP as a transchelating agent will be a simple and useful method for clinical application.

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