• Title/Summary/Keyword: RSD

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Coulometric Determination of Plutonium in PWR Spent Fuels (PWR 사용후핵연료내 플루토늄의 전기량적 정량)

  • Sohn, Se Chul;Suh, Moo Yul;Kim, Jung Suk;Song, Byung Chul;Jee, Kwang Yong;Choi,In Kyu;Kim, Won Ho
    • Journal of the Korean Chemical Society
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    • v.44 no.6
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    • pp.581-586
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    • 2000
  • Separation and coulometric titration method were applied for the determination of plutonium content in samples of PWR spent fuel. Plutonium was separated on an anion exchange(AG MP-1) column and determined by the controlled-potential coulometric titration. In this study, we discussed some experimental conditions related to the separation and determination of plutonium in PWR spent fuel samples. Average accuracy(recovery of plutonium) for the determination of 0.230∼3.02 mg plutonium standard was 99.36%. Average precision(relative standard deviation, RSD) for the determination of 0.250∼0.450 mg plutonium in PWR spent fuel samples was 0.38%.

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Comparative Study of Anti-osteoporotic Agents in Postmenopausal Women (골다공증 및 골감소증 치료제의 치료효과 비교연구)

  • Kim, Hee Sun;Sohn, Minji;Bang, Joon Seok;Sohn, Uy Dong
    • Korean Journal of Clinical Pharmacy
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    • v.24 no.2
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    • pp.98-105
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    • 2014
  • Purpose: The aim of this study was to compare retrospectively the efficacy of anti-osteoporotic agents (RAL-Raloxifene 60 mg, ALD-weekly alendronate 70 mg, RSD-weekly risedronate 35 mg, AVD3-weekly alendronate 70 mg/vitamin $D_3$ 2800IU, IBD-quarterly IV ibandronate 3 mg/3 ml, ZLD-yearly IV zoledronate 5 mg/100 ml) in postmenopausal patients with osteoporosis or osteopenia. Method: This study retrospectively reviewed medical record and compared the lumbar spine BMD percentage changes of each medicine group one year later from the baseline. 209 patients (27, 50, 60, 30, 35, and 7 patients in RAL, ALD, RSD, AVD3, IBD, and ZLD groups, respectively) are within the inclusion criteria for the study. Results: From baseline to month 12, lumbar spine BMD increased significantly larger with bisphosphonate groups, compared to SERM (p < 0.05). In all bisphosphonate groups, the lumbar spine BMD were increased significantly from baseline. Of the bisphosphonates, the changes from baseline in BMD of IV bisphosphonates were more larger than those of oral bisphosphonates, and yearly, quarterly bisphosphonates yielded significantly greater BMD gains, compared with weekly bisphosphonate groups (p<0.05). In addition, patients receiving 70 mg weekly alendronate+vitamin D3 had greater gains in BMD than alendronate Single preparation (p<0.05). Conclusion: Bisphosphonates yielded significantly greater BMD gains than SERM. Of the bisphosphonates, the changes from baseline in BMD of yearly, quarterly IV bisphosphonates yielded significantly greater BMD gains, compared with weekly oral bisphosphonate groups. In addition, vitamin D3 plays an significant role in BMD gains.

Evaluation of Endogeneous Steroids Profile after Administration of Anabolic Steroids (근육 강화제 복용에 의한 내인성 스테로이드 프로필 평가)

  • Lee, Seon Hwa;Choi, Man Ho;Kim, Tae Wook;Chung, Bong Chul
    • Journal of the Korean Chemical Society
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    • v.41 no.8
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    • pp.406-413
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    • 1997
  • The endogenous steroids from human urine were simultaneously analyzed by selected ion monitoring method of GC/MS which is currently used for the doping procedure, together with anabolic steroids. The recovery range of this method was 72.33 %∼94.54% and the RSD values of precision and accuracy test were 1.43%∼10.86%, 0.96%∼9.98%, respectively. Using this method steroids profile was investigated in the urine of male volunteers after oral administration of nine anabolic steroids banned by IOC (International Olympic Committee). Urinary endogenous steroids level was varied specifically according to the excretion tendency of the metabolites of anabolic steroids.

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Quantitative and Pattern Recognition Analyses for the Quality Evaluationof Herba Epimedii by HPLC

  • Nurul Islam, M.;Lee, Sang-Kyu;Jeong, Seo-Young;Kim, Dong-Hyun;Jin, Chang-Bae;Yoo, Hye-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.137-144
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    • 2009
  • In this study, quantitative and pattern recognition analyses for the quality evaluation of Herba Epimedii using HPLC was developed. For quantitative analysis, five major bioactive constituents, hyperin, epimedin A, epimedin B, epimedin C, and icariin were determined. Analysis was carried out on Capcell pak $C_{18}$ column ($250{\time}4.6$ mm, 5 ${\mu}m$) with a mobile phase of mixture of acetonitrile and 0.1% formic acid, using UV detection at 270 nm. The linear behavior was observed over the investigated concentration range (2-50 ${\mu}g/mL;\;r_2\;>$ 0.99) for all analytes. The intraand inter-day precisions were lower than 4.3% (as a relative standard deviation, RSD) and accuracies between 95.1% and 104.4%. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of one reference sample. The RSD of intra- and inter-day variation of relative retention time (RRT) and relative peak area (RPA) of the 12 selected common peaks were below 0.8% and 4.7%, respectively. The developed methods were applied to analysis of twenty Herba Epimedii extract samples. Contents of hyperin, epimedin A, epimedin B, epimedin C, and icariin were calculated to be 0$\sim$0.79, 0.69$\sim$1.91, 0.93$\sim$9.58, 0.65$\sim$3.05, and 2.43$\sim$11.8 mg/g dried plant. Principal component analysis (PCA) showed that most samples were clustered together with the reference samples but several apart from the main cluster in the PC score plot, indicating differences in overall chemical composition between two clusters. The present study suggests that quantitative determination of marker compounds combined with pattern-recognition method can provide a comprehensive approach for the quality assessment of herbal medicines.

A Study on the Comparison of Measuring Methods and Development of Emssion Factor on Mercury from Large-Scale Emission Sources (대형배출원에서의 수은 측정방법 비교 및 배출계수 개발에 관한 연구)

  • Kim, Hyung-Chun;Kim, Rhok-Ho;Kim, Jong-Hyeon;Lim, Seung-young;Kang, Dae-Il;Hong, Ji-Hyung;Jang, Kee-Won
    • Journal of Korean Society for Atmospheric Environment
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    • v.32 no.2
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    • pp.184-192
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    • 2016
  • Recently, studies on reducing mercury have been actively conducted worldwide, which include the current status of mercury emissions and mercury control technology. Among the control technology, Sorbent Trap measurement method has been aggressively developed due to its reliability, easiness in measurement and analysis. The purpose of this study is to evaluate the applicability of the new international measurement method; Sorbent Trap. For this, the study compared the Sorbent trap method (US EPA Method 30B) and the Korean Standard Method for Examination of Air (ES 01408.1) to evaluate their reliability, and developed mercury emission factors. As the result, the relative standard deviations (% RSD) of the two methods were 3.5~13.4% at Coal-fired Power Plants (CPP), 4.0~18.4% at Cement Kilns (CK), and 3.0~11.3% at Medical Waste Incinerators (MWI). The emissions factors were developed as 14.50 kg/ton at CPP, 45.10 kg/ton at CK, and 1,290.2 kg/ton at MWI.

Analysis Methods for Measurement of Ammonia Concentration (가스상 암모니아 측정을 위한 분석방법별 특성 연구)

  • Sa, Jae-Hwan;Yoon, Seok-Kyung;Roh, Gi-Hwan;Jeon, Eui-Chan
    • Journal of Korean Society for Atmospheric Environment
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    • v.24 no.1
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    • pp.43-54
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    • 2008
  • Management and control of ammonia at the sources and ambient largely depend on sampling and measurement techniques. Good sampling and measurement techniques provide high quality data. The main purpose of the study is compare the analytical characteristics of the Indolphenol method which is one of the standard method in Korea with automatic analyzers for continued measuring gaseous ammonia. For comparison with other analytical methods, the verification test was designed to evaluate performance parameters; linearity, absorption efficiency, reproducibility and repeatability test, accuracy, and response time test. $R^2$ of calibration curve using IPM and CLM was very high (value is 1.000), but for EcSM $R^2$ value was estimated to be lower than IPM and CLM (as 0.991). The RSD of the CLM ranged from 0.1 to 2.3% over the nine concentration levels measured, %Ds was 0.1 to 10.7%, and average RA over all the measurements was 3.3%. The RSD of IPM and EcSM was ranged from 1.0 to 8.1, 3.9 to 14.0 respectively, and average RA were 8.71, 4.9% respectively. Rise in response times of EcSM was estimated to be 1 minute. It is found to be more sensitive than response time (which ranged from 2 to 9 minute) of CLM. For ammonia concentration measured using the IPM and the CLM from the same ammonia source, linear regression of IPM versus CLM show a slope of 0.805, an intercept of 637 ppb, and $R^2$ of 0.868.

Quantitative analyses of ricinoleic acid and ricinine in Ricinus communis extracts and its biopesticides

  • Choi, Geun Hyoung;Kim, Leesun;Lee, Deuk Yeong;Jin, Cho long;Lim, Sung-Jin;Park, Byung Jun;Cho, Nam-Jun;Kim, Jin-Hyo
    • Journal of Applied Biological Chemistry
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    • v.59 no.2
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    • pp.165-169
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    • 2016
  • The quantitative analytical method for the bioactive substance, 3-cyano-4-methoxy-N-methyl-2-pyridone (ricinine) and an index compound, ricinoleic acid in castor plant (Ricinus communis) extract or oil was developed. For the determination of a pyridone alkaloid compound, ricinine, successive cartridge cleanup method combined with ultra-performance liquid chromatography was set up with $ENVI-Carb^{TM}$ (0.5 g) and $C_{18}$ SPE cartridges. Accuracy and precision were evaluated through fortification studies of one biopesticide (PE) at 10 and $100mg\;kg^{-1}$. Mean recoveries of ricinine were 98.7 and 96.0 % associated with less than 10 % RSD, respectively. For the determination of ricinoleic acid in castor extract and oil, saponification and methylation were optimized using gas chromatography-time of flight mass spectrometry. Recovery was more than 84.8 % associated with 6.2 % RSD after derivatization procedure. Both methodologies developed were applied to analyze real samples including three castor oil products and six commercially available biopesticides containing R. communis, collected at Korean market. The contents of ricinine and ricinoleic acid in most commercial biopesticides were less than the oil or extract contents indicated by label.

Simultaneous Determination of Paeoniflorin, Trans-cinnamic Acid, Schisandrin and Glycyrrhizin in So-Cheong-Ryong-Tang by HPLC-DAD and HPLC-ESI-MS

  • Lee, Mi-Kyeong;Lee, Ki-Yong;Park, Jung-Hyun;Kim, Seung-Hyun;Choi, Ok-Gyung;Park, Jin-Ho;Cho, Jung-Hee;Kim, Do-Hoon;Baek, Ju-Hyun;Oh, Mi-Hyune;Kim, Hyo-Jin;Sung, Sang-Hyun
    • Natural Product Sciences
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    • v.16 no.1
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    • pp.26-31
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    • 2010
  • High performance liquid chromatographic method with diode-array detection (HPLC-DAD) has been performed for the simultaneous determination of four marker constituents, paeoniflorin, trans-cinnamic acid, schisandrin and glycyrrhizin in traditional herbal medicinal preparation, So-Cheong-Ryong-Tang (SCRT). The presence of paeoniflorin, trans-cinnamic acid, schisandrin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard, UV spectrum and ESI mass spectrum. All four compounds showed good linearity ($r^2$ > 0.998) in a relatively wide concentration ranges. The RSD for intra-day and inter-day precision was less than 3% and the limits of detection (LOD) were less than 30 ng. The mean recovery of each compound was 94.1-113.0% with RSD values less than 3.0%. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial SCRT products.

Application of Laser Ablation Inductively Coupled Plasma Mass Spectrometry for Characterization of U-7Mo/Al-5Si Dispersion Fuels

  • Lee, Jeongmook;Park, Jai Il;Youn, Young-Sang;Ha, Yeong-Keong;Kim, Jong-Yun
    • Nuclear Engineering and Technology
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    • v.49 no.3
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    • pp.645-650
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    • 2017
  • This technical note demonstrates the feasibility of using laser ablation inductively coupled plasma mass spectrometry for the characterization of U-7Mo/Ale5Si dispersion fuel. Our measurements show 5.0% Relative Standard Deviation (RSD) for the reproducibility of measured $^{98}Mo/^{238}U$ ratios in fuel particles from spot analysis, and 3.4% RSD for $^{98}Mo/^{238}U$ ratios in a NIST-SRM 612 glass standard. Line scanning allows for the distinction of U-7Mo fuel particles from the Al-5Si matrix. Each mass spectrum peak indicates the presence of U-7Mo fuel particles, and the time width of each peak corresponds to the size of that fuel particle. The size of the fuel particles is estimated from the time width of the mass spectrum peak for $^{98}Mo$ by considering the scan rate used during the line scan. This preliminary application clearly demonstrates that laser ablation inductively coupled plasma mass spectrometry can directly identify isotope ratios and sizes of the fuel particles in U-Mo/Al dispersion fuel. Once optimized further, this instrument will be a powerful tool for investigating irradiated dispersion fuels in terms of fission product distributions in fuel matrices, and the changes in fuel particle size or shape after irradiation.

Optimization of 1D 1H Quantitative NMR (Nuclear Magnetic Resonance) Conditions for Polar Metabolites in Meat

  • Kim, Hyun Cheol;Ko, Yoon-Joo;Kim, Minsu;Choe, Juhui;Yong, Hae In;Jo, Cheorun
    • Food Science of Animal Resources
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    • v.39 no.1
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    • pp.1-12
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    • 2019
  • The objective of this study was to establish an optimized 1D $^1H$ quantitative nuclear magnetic resonance (qNMR) analytical method for analyzing polar metabolites in meat. Three extraction solutions [0.6 M perchloric acid, 10 mM phosphate buffer, water/methanol (1:1)], three reconstitution buffers [20 mM 3-morpholinopropane-1-sulfonic acid, 2-[4-(2-hydroxyethyl)piperazin-1-yl]ethanesulfonic acid, phosphate buffer], and two pulse programs (zg30, noesypr1d) were evaluated. Extraction with 0.6 M perchloric acid and 20 mM phosphate resulted in a stable baseline and no additional overlap for quantifying polar metabolites in chicken breast. In qNMR analysis, zg30 pulse program (without water-suppression) showed smaller relative standard deviation (RSD) and faster running time than noesypr1d (water-suppression). High-performance liquid chromatography was compared with qNMR analyses to validate accuracy. The zg30 pulse program showed good accuracy and lower RSD. The optimized qNMR method was able to apply for beef and pork samples. Thus, an optimized 1D $^1H$ qNMR method for meat metabolomics was established.