• Nuclear Engineering and Technology
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• 제31권5호
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• pp.445-454
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• 1999

This work describes the adaptation of extractive scintillation by URAE $X^{TM}$ with a photon-electron rejecting alpha liquid scintillation (PERAL $S^{)}$ spectrometer to the analysis of uranium in aqueous samples. The extraction efficiency of the system was evaluated under varing chemical conditions including pH, and sample-cocktail volume ratio. Isotopic information from the (PERAL $S^{)}$ spectrum of natural uranium was obtained using a curve fitting routine. Comparisons of the result with that obtained from alpha spectrometry method using ion implanted silicon detector showed good agreement.t.

• Journal of Radiation Protection and Research
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• 제43권3호
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• pp.120-123
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• 2018

Background: Analysis of enrichment of $UO_2$ is important to verify the information declared by the license-holders. The redundancy methods are required to guarantee the analysis result. Korea Institute of Nuclear Nonproliferation and Control (KINAC) used to analyze it with alpha spectrometry and consign to Korea Basic Science Institute (KBSI) Thermal Ionization Mass Spectrometry (TIMS). This article evaluated the similarity of the results with two methods and derive correlation equation. It could be compared to the results measured by TIMS running by KBSI. Materials and Methods: There are not many certified materials for the uranium enrichment value. Therefore, 34 uranium pellets, which have the wide range of uranium enrichment from 0.21 to 4.69 wt%, were used for the experiments by the alpha spectrometry and the TIMS. Results and Discussion: The study shows there are the tendency of analyzed enrichment by each equipment. It shows uranium enrichment with alpha spectrometry evaluated 17% higher than that with TIMS on average. The regression equations were also derived in case the similarity between the two results with two methods is lower than predicted. Two experiments were designed to compare the effect of number of samples. The $R^2$ was 0.9977 with 34 pellets. It shows the equation is appropriate to predict the enrichment values by TIMS with that of alpha spectrometry. The $R^2$ was 0.9858 with four pellets for ten times. The $R^2$ decreased while the number of samples increased. The discrepancy between the lowest and highest enrichment seems to be one of the reason for it. Conclusion: KINAC expects the first equation with 34 samples is useful to predict the result with TIMS, the redundancy method, based on the alpha spectrometry. The extra samples are necessary to collect if the enrichment value analyzed by TIMS is lower than the value predicted with the equation. Further study would be followed related to the impact of the peak counts for each uranium isotopes, sample amount and number of experiments when TIMS established in KINAC by the end of 2018.

• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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• pp.214.1-214.1
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• 2003

Metabonomic analysis using Liquid Chromatography-Mass Spectrometry (LC-MS) was employed to test the feasibility to predict chemical-induced toxicity. Time-dependent metabolic variations were evaluated in rats treated with the model hepatotoxin, ${\alpha}$- naphthylisothiocyanate (ANIT). Urine samples of ANIT treated group and control group were collected up to 7 days postdose. Urine samples were analyzed by gradient HPLC combined with electrospray mass spectrometry. The chromatographic results were data-reduced and analyzed using principal component analysis to show the time dependent biochemical variations induced by ANIT toxicity. (omitted)

• 분석과학
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• 제13권5호
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• pp.549-557
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• 2000

자외선/가시선 영역에서 뚜렷한 발색단이 없는 화합물 수용액의 반응을 추적하기 위해 FTIR-ATR 분광법이 사용되었다. 구체적인 예로서, 산성 수용액에서 ${\alpha}$-사이클로덱스트린과 ${\gamma}$-사이클로덱스트린의 가수분해 반응을 FRIR-ATR 분광법으로 연구하였다. 각각 1.0M, 0.5M, 0.1M 농도의 HCl 조건에서 두 사이클로덱스트린의 가수분해 반응을 연구한 결과, 강한 산성 용액에서 ${\alpha}$-사이클로덱스트린의 가수분해 생성물은 글루코오스이지만 ${\gamma}$-사이클로덱스트린의 가수분해 생성물은 글루코오스에서 더욱 분해된 물질이었다.

• 대한화학회지
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• 제27권4호
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• pp.279-286
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• 1983

몇가지의 알파입자를 방출하는 핵종, 즉 악티늄족 원소들, $^{207}Bi$ and $^{210}Po$을 전해석출하는 장치를 만들었다. 스텐레스 원판으로된 환원전극에 이 동위원소들을 석출했으며(석출부분 직경=18mm), 산화전극으로는 백금선을 썼다. 전해질로 염화암모늄을 쓰고, 초기 pH=4, 염소이온농도=0.6M이하, 용액부피=15ml로 하여 1.5암페어(전류밀도=0.59A/$cm^2$)의 전류를 100분간 흘려주어 98.3%의 석출 회수율과 ${\pm}$0.7%의 재현도를 얻었다. 석출된 시료의 알파스펙트럼을 측정한 결과 에너지 분리도로서 $^{210}Po=18.3keV, ^{234}U=21.8keV$ 및 $^{239}Pu=36.0keV$인 반치전폭(full width at half maximum)을 얻었다. 국산 천연우라늄(충북·괴산) 시료를 전해석출하여 그의 알파스펙트럼을 구한 결과 $^{238}U\;:\;^{234}U\;=\;:\;6.1{\times}10^{-5}$을 얻었으며 $1.8{\sim}10^{13} neutrons/cm^2{\cdot}sec$인 중성자속으로 144일 동안 쪼여준 238U 시료를 전해석출하여 그의 알파스펙트럼을 구한 결과 $^{238}U\;:\;^{239}Pu\;:\;241Am\;=\;100\;:\;0.0263\;:\;5.20{\times}10^{-5}$을 얻었다. 조사시료중의 $^{238}U$에 대한 본실험의 정량결과는 고체형광측정법 및 질량 스펙트럼법에 의한 결과들과 상대오차 1.6% 이내에서 일치하였으며, $^{239}Pu$의 경우는 음이온교환분리-알파스펙트럼 측정 및 삼불화테노일아세톤(thenoyltrifluoroacetone)을 쓴 용매추출-알파스펙트럼 측정에 의한 정량결과들과 상대오차 ${\pm}$4.0%이내에서 일치하였다.

• Bulletin of the Korean Chemical Society
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• 제26권9호
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• pp.1347-1353
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• 2005

Sets of sialic acid-containing trisaccharides having different internal and terminal linkages have been synthesized to develop a sensitive method for analysis of the reducing terminal linkage positions. The trisaccharides, sialyl($\alpha$ 2-3)Gal($\beta$ 1-3)GalNAc and sialyl($\alpha$ 2-3)Gal($\beta$ 1-X)GlcNAc where X=3, 4 and 6, were synthesized and examined using electrospray ionization (ESI)-collision induced dissociation (CID) tandem mass spectrometry (MS/MS). The compounds chosen for this study are related to terminal groups likely to be found on polylactosamine-like glycoproteins and glycolipids which occur on the surface of mammalian cells. The purpose of this study is to develop tandem mass spectrometral methods to determine detailed carbohydrate structures on permethylated or partially methylated oligosaccharides for future applications on biologically active glycoconjugates and to exploit a faster method of synthesizing a series of structural isomeric oligosaccharides to be used for further mass spectrometry and instrumental analysis.

• Mass Spectrometry Letters
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• 제6권1호
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• pp.7-12
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• 2015

In the present study, we proposed a simple ESI-MS model for determining $Zn^{2+}$ binding (or dissociation) constants for zinc finger peptides (ZFPs) with a unique ${\beta}{\beta}{\alpha}$ fold consensus. The ionization efficiency (response) factors for this model, i.e., ${\alpha}$ and ${\beta}$, could be determined for ZiCo ZFP with a known $Zn^{2+}$ binding constant. We could determine the binding constants for other ZFPs assuming those with a ${\beta}{\beta}{\alpha}$ consensus conformation have the same ${\alpha}/{\beta}$ response ratio. In general, the ZPF dissociation constants exhibited $K_d$ values of $10^{-7}{\sim}10^{-9}M$, while $K_d$ values for a negative control non-specific $Zn^{2+}$ peptides were high, e.g., $5.5{\times}10^{-6}M$ and $4.3{\times}10^{-4}M$ for BBA1 and melittin, respectively.

• Mass Spectrometry Letters
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• 제3권1호
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• pp.21-24
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• 2012

$5{\alpha}$-Dihydrotestosterone (DHT) is the primary active metabolite of testosterone, catalyzed by $5{\alpha}$-reductase ($5{\alpha}R$) in the skin, prostate, and liver. In this study, the $5{\alpha}R$ activity in rat liver S9 fraction in the presence of a NADPH-generating system was evaluated and compared by gas chromatography-mass spectrometry (GC-MS)-based in vitro assays. Testosterone and a $5{\alpha}R$ inhibitor, finasteride, were added to the S9 fractions and incubated at $37^{\circ}C$ for 1 h. Both testosterone and DHT were quantitatively measured and compared with two different GC-MS-based steroid profiling techniques. DHT was not detected by conventional GC-MS analysis in the absence of finasteride when the concentration of testosterone in the S9 fraction was less than $0.2{\mu}M$, whereas the isotope-dilution GC-MS (GC-IDMS) system was able to evaluate the $5{\alpha}R$ activity. Because the S9 fraction contains more reactive enzymes and is easier to collect from tissues compared with a microsomal solution, the combination of the S9 fraction and GC-IDMS technique may be a promising assay for evaluating the $5{\alpha}R$ activity in large-scale clinical studies.

• Bulletin of the Korean Chemical Society
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• 제24권5호
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• pp.657-660
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• 2003

• 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.