• Title/Summary/Keyword: Method detection limits

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Simultaneous Determination of Haloperidol and Its Metabolite, Reduced Haloperidol, in Plasma by Gas Chromatography Using Nitrogen Phosphorous Selective Detection (Gas Chromatography-Nitrogen Phosphorous Selective Detection을 이용한 혈장중 Haloperidol 및 대사체인 Reduced Haloperidol의 동시정량)

  • Park, Kyoung-Ho;Lee, Min-Hwa;Shim, Chang-Koo;Lee, Myung-Gull;Park, Jong-Sei
    • Journal of Pharmaceutical Investigation
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    • v.22 no.3
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    • pp.197-204
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    • 1992
  • A gas chromatographic method using nitrogen phosphorous selective detection was developed for simultaneous determination of haloperidol and its metabolite, reduced haloperidol, in human plasma. Combelen was used as internal standard, The method involved extraction and trimethylsilylation followed by the injection of $2-4\;{\mu}l$ of benzene layer, which was used to dissolve the trimethylsilylated derivatives of haloperidol and reduced haloperidol, onto SE-54 column [5% phenyl methyl silica fused capillary column, $16m{\times}0.22\;mm$ $(I.D.){\times}0.33\;{\mu}m$ (coated thickness)]. The temperature of column oven was programmed from $200^{\circ}C\;to\;300^{\circ}C$ at the increase rate of $10^{\circ}C/min and also the temperatures of injector and detector were set at $300^{\circ}C$. Helium was used as carrier gas and its flow rate was maintained at 30 ml/min. The detection was conducted with nitrogen phosphorous selective detector. The retention times for combelen, reduced haloperidol and haloperidol were found to be 9.14, 9.75 and 9.99 min, respectively. The detection limits for haloperidol and reduced haloperidol in human plasma were both 0.2 ng/ml. The coefficients of variation of the intra-assay were generally low (below 9.8%). The mean absolute recoveries of added haloperidol and reduced haloperidol from plasma were 72% and 84%, respectively. No interferences from endogenous substances were found.

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A Study on Improved Detection Signature System in Hacking Response of One-Line Games (온라인 게임 해킹대응에서 Signature 기반 탐지방법 개선에 관한 연구)

  • Lee, Chang Seon;Yoo, Jinho
    • The Journal of Society for e-Business Studies
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    • v.21 no.1
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    • pp.105-118
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    • 2016
  • Game companies are frequently attacked by attackers while the companies are servicing their own games. This paper analyzes the limit of the Signature detection method, which is a way of detecting hacking modules in online games, and then this paper proposes the Scoring Signature detection scheme to make up for these problems derived from the limits. The Scoring Signature detection scheme enabled us to detect unknown hacking attacks, and this new scheme turned out to have more than twenty times of success than the existing signature detection methods. If we apply this Scoring Signature detection scheme and the existing detection methods at the same time, it seems to minimize the inconvenient situations to collect hacking modules. And also it is expected to greatly reduce the amount of using hacking modules in games which had not been detected yet.

Determination of MTBE, TBA and BTEX in Soil by Headspace Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1693-1698
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    • 2012
  • A headspace gas chromatographic mass spectrometric (GC-MS) assay method was developed for the simultaneous determination of methyl tertiary butyl ether (MTBE), $tert$-butyl alcohol (TBA) and benzene, toluene, ethyl benzene and xylene (BTEX) in soil contaminated with gasoline. 2 g of soil sample were placed in a 10 mL headspace vial filled with 5 mL of phosphoric acid solution (pH 3) saturated with NaCl, and the solution was spiked with fluorobenzene as an internal standard and sealed with a cap. The vial was heated in a heating block for 40 min at $80^{\circ}C$. The detection limits of the assay were 0.08-0.12 ${\mu}g$/kg for the analytes. For five independent determinations at 10 and 50 ${\mu}g$/kg, the relative standard deviations were less than 10%. The method was used to analyze fifty six soil samples collected from various regions contaminated with gasoline in Korea. The developed method may be valuable for the monitoring of the analytes in soil.

Simultaneous Analytical Method of Organochlorine and Pyrethroid Pesticides using GC(ECD) (GC-ECD를 이용한 유기염소계 밑 Pyrethroid계 농약 동시 분석법)

  • 김우성;이선화;김재이;정지윤;이명자;박영채;이영자;정성욱;이봉헌
    • Journal of Environmental Science International
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    • v.12 no.4
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    • pp.477-480
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    • 2003
  • Pesticides were extracted from samples with 70% acetone and methylene chloride in order, and then cleaned up via open-column chromatography apparatus packed with florisil, and finally analyzed simultaneously the organochlorine and pyrethroid pesticides using GC(ECD). An ultra-2 fused silica capillary column was used to separate and identify the products. The resolution between the last isomeric peak of cypermethrin(59.987min) and the first isomeric peak of flucythrinate(60.043min) was not satisfactory. The last isomeric peak of fenvalerate(62.344min) and the first isomeric peak of fluvalinate(62.397min) were overlapped. Recoveries of soybean sample fer the most pesticides were 73.3% to 102.4%. Detection limits were between 0.004 and 0.063 ${\mu}$g/mg when this method was used.

Measurement and Compensation of Nonlinearity in Homodyne Interferometer (Homodyne 간섭계에서의 비선형성 측정과 보정)

  • Kim, Jong-Yun;Eom, Tae-Bong;Jeong, Kyu-Won;Choi, Tae-Young;Lee, Keon-Hee
    • Journal of the Korean Society for Precision Engineering
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    • v.18 no.9
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    • pp.171-178
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    • 2001
  • The nonlinearity of a laser interferometer usually ranges from sub-nanometer to several manometers. This nonlinearity, which has periodic characteristics, limits the accuracy of the interferometer at the sub-nanometer level. The nonlinearity error of the one-frequency homodyne interferometer with quadrature fringe detection results from a number of factors including polarization mixing by imperfect optical elements, unequal gain of photo detectors, lack of quadrature between two signals and misalignment. In this paper, we described a method for measuring and compensating the nonlinearity of homodyne interferometer using the elliptical fitting technique with least-square method. Experimental results demonstrate that $^\pm$3.5 nm nonlinearity can be reduced to $^\pm$0.2 nm level.

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A Study on Analytical Method of Phthalate Esters in Water by SPE(Solid-Phase-Extraction) (고체상 추출법을 이용한 Phthalate Esters의 분석방법 연구)

  • 홍성희;한개희;이찬형;이순화
    • Journal of Environmental Science International
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    • v.12 no.1
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    • pp.81-86
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    • 2003
  • The study was carried out to evaluate the new analytical method of phthalate esters(diethylphthalate, di-n-butylphthalate, butylbenzylphthalate, bis(2-ethylhexyl)phthalate), one of the endocrine disruptors, which were performed by GC/MS-SIM(selected ion monitoring). The phthalate esters were extracted from water samples using solid-phase extraction on $C_{18}$ columns. It investigated that the extraction recovery rate of phthalate esters with different solvents and solvent volume. The optimal solvent was dichloromethane and proper volume of dichloromethane for recovery of phthalate esters was 4 mL. There were good linearities(above $R^2$=0.9975) in the range 0.01~0.50mg/L, and the detection limits were below 0.01~0.03$\mu\textrm{g}$/L. The recovery rates, RSD and MDLs for phthalate esters were 80~114%, 5.0~8.1% and 0.03~0.11$\mu\textrm{g}$/L, respectively. This method shows a good precision of phthalate esters.

Simultaneous Determination of 285 Chemicals in Water at ppt Levels by GC-Ion Trap Mass Spectrometry

  • Kadokami, Kiwao;Sato, Kenji;Koga, Minoru;Shinohara, Ryota
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.771-778
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    • 1995
  • The authors have developed an analytical method for determining trace amounts of 285 kinds of chemicals in natural waters by GC-ion trap MS. The results of overall recovery tests at $0.1{\mu}g/l$ showed that the mean recovery was 92.1% and the mean relative standard deviation was 10.8%. The mean of the method detection limits was $0.036{\mu}g/l$. From the results of analysis of real samples, it was confirmed that this method is useful to elucidate the concentration levels and the fate of chemicals in the aquatic environment.

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Evaluation of an Ammonia Passive Sampler Using Chamber System

  • Yim, Bong-Been;Kim, Sun-Tae
    • Journal of Korean Society for Atmospheric Environment
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    • v.22 no.E1
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    • pp.1-8
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    • 2006
  • The purpose of this study was to evaluate the efficiency of a passive sampler in measuring atmospheric ammonia concentrations using chamber system. The ability of the passive sampler to quantitatively determine atmospheric ammonia gas was almost identical to that of the reference method (indophenol method). There was no significant difference between concentrations measured by the two methods. The detection and quantification limits of the ammonia passive sampler were 16.9 ppb and 25.3 ppb, respectively, for a 24-h sampling period. The average coefficient of variation between replicated samplers was $6.7{\pm}4.2%$. The concentrations measured by the two methods (passive sampler and indophenol method) were no significant difference with good a correlation (correlation coefficient=0.964).

A new sensitive determination method of propylene oxide-hemoglobin adducts by EI-GC-MS (SIM)

  • Shin, Ho-Sang;Lee, Jin-Heon;Ahn, Hye-Sil
    • Proceedings of the Korean Environmental Health Society Conference
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    • 2004.06a
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    • pp.169-172
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    • 2004
  • A gas chromatography/mass spectrometric assay method was developed for the determination of propylene oxide adduct, N-(3-hydroxypropyl)valine. Adduct was released from hemoglobin by alkaline hydrolysis and extract at pH 8 with ethyl ether. The dried extract was completely derivatized with N-Methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA)/TMS-I (100:3). The detection limits of the assay were 0.08 ng/g for N-(3-hydroxypropyl)valine based upon assayed hemoglobin of 0.1 g. The method was applied to the determination of propylene oxide adduct formed in young female Sprague-Dawley rats after treatment for 1, 2 and 3 weeks with 0.008 % propylene oxide via the drinking water. An adduct was detected by proposed procedure. The structure of the adduct could be assigned to N-(3-hydroxypropyl)valine.

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A study on determination of carbadox and olaquindox in swine tissues by matrix solid Phase disperse method" (MSPD 방법에 의한 돈육중 Carbadox와 Olaquindox 분석법 연구)

  • 황래홍;김영수;김기근
    • Korean Journal of Veterinary Service
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    • v.19 no.2
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    • pp.163-171
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    • 1996
  • This study was carried out to determination of carbadox and olaquindox residues in swine tissues by MSPD(matrix solid phase disperse)method. The results obtained were as follows ; 1. Optimal wavelengths of UV for carbadox and olaquindox were 310 and 370nm, respectively 2. Ethyl acetate-Acetonitrile(8:2) was found to be adequate as extractant in this method. 3. The average overall recovery of carbadox at the 0.01, 0.05, and 1.0PPM spike levels was 89. 2% and that of olaquindox was 89.9%, and the detection limits were 0.5ng for carbadox and olaquindox.

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