• 제목/요약/키워드: Detection limits

검색결과 934건 처리시간 0.03초

Rapid Determination of Chlorostyrenes in Fish by Freezing-Lipid Filtration, Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry

  • Kim, Min-Sun;Park, Kwang-Sik;Pyo, Hee-Soo;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • 제29권2호
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    • pp.352-356
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    • 2008
  • An analytical method has been developed for measuring chlorostyrenes in fish tissue sample. Extraction of chlorostyrenes from fish tissue was carried out by ultrasonication using acetone/n-hexane (5:2, v/v) mixture. Most of the lipids in the extract were eliminated by freezing-lipid filtration, prior to solid-phase extraction (SPE) cleanup. During freezing-lipid filtration, about 90% of the lipids extracted from the fish samples were easily removed without any significant losses of chlorostyrenes. For purification, SPE using Florisil was used for the rapid and effective cleanup. Quantification was performed using gas chromatography-mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery was above 80% in the spiked fish tissue sample at 10 and 100 ng/g levels, respectively. The detection limits for chlorostyrenes were ranged from 0.05 to 0.1 ng/g. This developed method is demonstrated to give efficient recoveries and LODs for detecting chlorostyrenes spiked into fish tissue with high lipid content.

Rapid and Simultaneous Determination of Volatile Fatty Acids and Indoles in Pig Slurry and Dog Excrement by Solid-Phase Micro-Extraction Method with Gas Chromatography

  • Kim, Hyun-Jung;Yu, Mee-Seon;Yang, Sung-Bong
    • 한국환경과학회지
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    • 제23권10호
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    • pp.1693-1701
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    • 2014
  • A rapid and simple method for the quantitative determination of volatile fatty acids (VFAs; propionic acid, n-butyric acid, i-valeric acid and n-valeric acid) and indoles (phenol, p-cresol, 4-ethyl phenol, indole and skatole) in pig slurry and dog excrement using solid-phase micro-extraction (SPME) coupled to gas chromatography was evaluated. $50/30{\mu}m$ DVB/CAR/PDMS (Divinylbenzene/Carboxen/Polydimethylsiloxane) fiber was used to extract the target compounds in aqueous media. Sample amount and adsorption time was standardized for the routine analysis. Detection limits were from 0.11 to $0.15{\mu}gL$ for VFAs and from 0.12 to $0.28{\mu}gL$ for indoles and the correlations observed ($R^2$) were 0.975~1.000. This method was applied to the pig slurry, fertilizer, compost and dog excrement. In nearly all cases, the indoles were detected in concentrations of higher than their limits of detection (DOLs). But the VFAs in swine manure were below their DOLs.

Determination of Acaricides in Honey by Solid-Phase Extraction and Gas Chromatography / Mass Spectrometry

  • Hong, Joo-Yeon;Jung, Ok-Sang;Ryoo, Jae-Jeong;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • 제30권1호
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    • pp.61-66
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    • 2009
  • An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

Airborne HPGe spectrometer for monitoring of air dose rates and surface activities

  • Marcel Ohera;Lubomir Gryc;Irena Cespirova;Jan Helebrant;Lukas Skala
    • Nuclear Engineering and Technology
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    • 제55권11호
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    • pp.4039-4047
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    • 2023
  • This contribution describes the application of HPGe detector for the airborne quantitative analysis. The hardware of the airborne HPGe system was designed from the commercial components with only exception of the newly designed AirHPGeSpec special software to control, measure and process the data. The system was calibrated for the local air kerma rates measured on helicopter board and its conversion to the air kerma rates at 1 m above the ground was proposed. Two examples of the air kerma rates measured over the former uranium mining areas are presented and compared with the results of other airborne system on the board. This airborne HPGe system could be also used for measuring the surface activities in a radiation event. The nuclides of 131I, 132Te - 132I, 133I, 134I, 135I, 137Cs, 134Cs, 88Rb and 103Ru were selected from possible nuclear power plant emergency scenarios. The Monte Carlo simulation was used to calculate HPGe detector efficiencies for the flight altitudes from 25 to 300 m for the energies from 300 keV to 3 MeV of the nuclides in question. Also, the detection limits according to the Currie method as well as ISO 11929-2010 for selected nuclides are presented.

유전자 변형 작물 성분 검출용 PCR Kit의 성능 평가 연구 (Performance Evaluation of PCR Kits for Detecting Genetically Modified Crop Ingredients)

  • 윤시온;정순천;윤원기;박상규;문제선;이정현;김환묵
    • Toxicological Research
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    • 제20권2호
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    • pp.101-108
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    • 2004
  • 유전자변형작물의 이점과 잠재적 위해에 관한 다른 사회적 인식은 각국에서 다른 반응을 유발시켜왔다 한국을 포함한 많은 국가는 새로운 규제를 제정하기 위해 부심하고 있다 한국은 최근에 3% 이상의 유전자변형작물 혼입을 포함하는 모든 식품에 표시제를 실시하였다. 유전자변형작물 혼입을 신속하고 간편하게 검출하는 방법의 하나는 PCR에 의한 도입 DNA의 증폭이다 이 목적을 위한 많은 PCR kit가 시판되고 있어, 본 연구는 이들 상업화된 유전자변형작물 검출 kit의 성능을 시험하였다. 그 결과 이들 15개 kit 중 6개는 안정성, 재현성 및 검출 한계의 측면에서 제작사 스스로 제시한 요구조건도 충족하지 못하여 이들 kit의 개발 및 생산 단계에서 품질관리에 문제점이 있음을 시사하였다 본 시험은 또한 duplex와 triplex검출 kit가 단일 PCR 반응에서 명백한 검출을 보장할지라도, monoplex 검출 kit의 검출 능력이 가장 높다는 것을 시사하였다. 또한, kit들은 콩과 옥수수 사이에서 다른 검출 한계를 보였다. 본 연구의 결과는 GM 작물의 재배, 국가간 이동, GM 작물을 사용한 식품 생산 과정의 모니터링 뿐만 아니라 GM작물과 관련한 정부의 법규를 준수하기 위한 GM작물의 혼입의 건전한 과학적 추적체계의 개발에 유용할 것이라 사료된다.

PREDICTION OF THE DETECTION LIMIT IN A NEW COUNTING EXPERIMENT

  • Seon, Kwang-Il
    • 천문학회지
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    • 제41권4호
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    • pp.99-107
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    • 2008
  • When a new counting experiment is proposed, it is crucial to predict whether the desired source signal will be detected, or how much observation time is required in order to detect the signal at a certain significance level. The concept of the a priori prediction of the detection limit in a newly proposed experiment should be distinguished from the a posteriori claim or decision whether a source signal was detected in an experiment already performed, and the calculation of statistical significance of a measured source signal. We formulate precise definitions of these concepts based on the statistical theory of hypothesis testing, and derive an approximate formula to estimate quickly the a priori detection limit of expected Poissonian source signals. A more accurate algorithm for calculating the detection limits in a counting experiment is also proposed. The formula and the proposed algorithm may be used for the estimation of required integration or observation time in proposals of new experiments. Applications include the calculation of integration time required for the detection of faint emission lines in a newly proposed spectroscopic observation, and the detection of faint sources in a new imaging observation. We apply the results to the calculation of observation time required to claim the detection of the surface thermal emission from neutron stars with two virtual instruments.

Ex Vivo Assay of Trace Nicotine Using a Voltammetric Modified Biosensor

  • Ly, Suw Young;Jang, Myung-Ho;Cha, Jae-Min;Kim, Min-Young;Oh, Hyun-Seok;Jo, Dong-Hyeon;Choi, Seong-Sik
    • 한국응용과학기술학회지
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    • 제29권1호
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    • pp.40-46
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    • 2012
  • In vivo nicotine is associated with Alzheimer's, Parkinson's and lung cancer. Diagnostic assays of these diseases depend on very low analytical detection limits. In this study, a sensitive analytical method was examined using a voltammetric graphite pencil electrode (GPE) and a modified carbon nanotube paste electrode (CNE). The optimum analytical conditions for both electrodes were compared using square wave anodic stripping voltammetry (SW) and cyclic voltammetry (CV) obtaining 400 sec accumulation time and oxidation peak. Under optimum parameters, the stripping working range of GPE was $5.0-40.0{\mu}g/L$, CNE: 0.1-0.8 and $5-50{\mu}g/L$. Quantification limits were $5.0{\mu}g/L$ for GPE and $0.1{\mu}g/L$ for CNE, while detection limits were $0.6{\mu}g/L$ for GPE and $0.07{\mu}g/L$ for CNE. A standard deviation of $10.0{\mu}g/L$ was observed for 0.064 GPE and 0.095 CNE (n = 12) using 400 sec accumulation time. The results obtained can be applied to non.treated urine and ex vivo biological diagnostics.

Lower the Detection Limits of Accelerator Mass Spectrometry

  • ;송종한;김준곤;김재열;오종주;김종찬
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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    • pp.243-244
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    • 2013
  • Over the past 15 years, several groups have incorporated radio-frequency quadrupole (RFQ) based instruments before the accelerator in accelerator mass spectrometry (AMS) systems for ion-gas interactions at low kinetic energy (<40 eV). Most AMS systems arebased on a tandem accelerator, which requires negative ions at injection. Typically, AMS sensitivity abundance ratios for radioactive-to-stable isotope are limited to Xr/Xs >10^-15, and the range of isotopes that can be analyzed is limited because of theneed to produce rather large negative ion beams and the presence of atomic isobaric interferences after stripping. The potential of using low-kinetic energy ion-gas interactions for isobar suppression before the accelerator has been demonstrated for several negative ion isobar systems with a prototype RFQ system incorporated into the AMS system at IsoTrace Laboratory, Canada (Ontario, Toronto). Requisite for any such RFQ system applied to very rare isotope analysis is large transmission of the analyte ion. This requires proper phase-space matching between the RFQ acceptance and the ion beam phase space (e.g. 35 keV, ${\varphi}3mm$, +-35 mrad), and the ability to control the average ion energy during interactions with the gas. A segmented RFQ instrument is currently being designed at Korea Institute for Science and Technology (한국과학기술연구원, KIST). It will consist of: a) an initial static voltage electrode deceleration region, to lower the ion energy from 35 keV down to <40 eV at injection into the first RFQ segment; b) the segmented quadrupole ion-gas interaction region; c) a static voltage electrode re-acceleration region for ion injection into a tandem accelerator. Design considerations and modeling will be discussed. This system should greatly lower the detection limits of the 6 MV AMS system currently being commissioned at KIST. As an example, current detection sensitivity of 41Ca/Ca is limited to the order of 10^-15 while the 41Ca/Ca abundance in modern samples is typically 41Ca/Ca~10^-14 - 10^-15. The major atomic isobaric interference in AMS is 41K. Proof-of-principal work at IsoTrace Lab. has demonstrated that a properly designed system can achieve a relative suppression of KF3-/41CaF3- >4 orders of magnitude while maintaining very high transmission of the 41CaF3- ion. This would lower the 41Ca detection limits of the KIST AMS system to at least 41Ca/Ca~10^-19. As Ca is found in bones and shells, this would potentially allow direct dating of valuable anthropological archives and archives relevant to our understanding of the most pronounced climate change events over the past million years that cannot be directly dated with the presently accessible isotopes.

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False Alarm Rate 변화에 따른 DoS/DDoS 탐지 알고리즘의 성능 분석 (Performance Analysis of DoS/DDoS Attack Detection Algorithms using Different False Alarm Rates)

  • 장범수;이주영;정재일
    • 한국시뮬레이션학회논문지
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    • 제19권4호
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    • pp.139-149
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    • 2010
  • 인터넷은 확장성과 최선형 라우팅 서비스를 목적으로 설계되었기 때문에 보안상에 취약점을 가진다. 이에 IP spoofing과 DoS/DDoS 공격을 탐지하기 위한 다양한 공격 탐지 방법들이 제안되었다. DoS/DDoS 공격은 공격이 시작되고 짧은 시간 내에 목적을 이루기 때문에 공격 탐지 알고리즘들은 빠른 시간 내에 정확한 탐지를 하는 것이 중요하다. 공격 탐지 알고리즘들은 미탐지율과 오탐지율로 이루어진 오경고율을 가지며 공격 탐지 알고리즘의 성능을 평가하는 중요한 요소가 된다. 본 논문에서는 공격 탐지 알고리즘의 특징을 살펴보고 그 성능을 분석하였다. 공격 탐지 알고리즘의 성능은 미탐지율과 오탐지율을 변화시켰을 시, 공격 트래픽 및 일반 트래픽에 미치는 영향을 시뮬레이션을 통해 각각 분석하였다. 이를 통해 전송되는 공격 패킷의 수는 미탐지율에 비례하며, 전송되는 일반 패킷의 수는 일정 치 이하의 미탐지율과 오탐지율에 반비례하는 것을 확인하였다. 또 공격 탐지 알고리즘의 미탐지율 변화에 따른 오탐지율의 변화를 분석하여 미탐지율과 오탐지율의 관계를 도출하고 공격탐지 알고리즘의 한계를 분석하였다. 이러한 한계를 극복하기 위해 정확한 네트워크 상태를 판단하여 공격 탐지 알고리즘의 한계를 줄이고 성능을 개선하는 방안을 제안하였고 그 결과, 공격 탐지 알고리즘의 성능이 보다 향상됨을 확인하였다.

서울지역 유통 식육 중의 세팔로스포린계 항균물질 잔류실태 조사 (Monitoring for cephalosporins residues in raw meat in Seoul)

  • 김미란;최윤화;최훈;김두환;김영섭;이주형
    • 한국동물위생학회지
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    • 제38권4호
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    • pp.259-264
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    • 2015
  • We investigated the residues of 6 cephalosporins (cefquinome, cephalexin, cephalonium, cefazolin, ceftiofur, cefuroxime) using LC-MS/MS in raw meat in Seoul. This method involves extraction of the residue from the meat by distilled water and methanol followed by a manual of residue analysis published by the National Institute of Food and Drug Safety Evaluation. The recoveries ranged between 74.71~90.01% in beef, 73.37~101.40% in pork and 70.87~95.53% in chicken, respectively. The limits of detection were 0.0004~0.0563 mg/kg, and the limits of quantification were 0.001~0.169 mg/kg respectively. Residues of cephalosporins which exceeded maximum residue limits (MRL) were not exceed in any of the 287 samples. However, it is necessary to develop multi-method, which includes the active metabolites of ceftiofur.