• 제목/요약/키워드: Analytical mode

검색결과 933건 처리시간 0.021초

동위원소희석 액체크로마토그래피-질량분석법을 이용한 육류 중 클로람페니콜의 정밀한 정량 분석에 관한 연구 (Accurate determination of chloramphenicol in meat by isotope dilution liquid chromatography mass spectrometry (ID-LC/MS))

  • 송혜민;김병주;정혁;안성희
    • 분석과학
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    • 제23권6호
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    • pp.524-530
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    • 2010
  • 클로람페니콜은 미생물과 박테리아들의 활동을 억제시킴으로써 동물 치료에 효과적인 축산 항생제 중의 하나이다. 그러나 사람에게 재생 불량성 빈혈과 같은 치명적인 부작용이 발생하여 식용으로 사육하는 동물들에 대한 클로람페니콜의 사용을 유럽을 포함한 많은 나라에서 금지하였다. 본 연구에서는 돼지고기 시료 중 클로람페니콜을 분석하기 위하여 동위원소희석 액체크로마토그래피-질량분석법(IDLC/MS/MS)을 이용하여 정확하고 정밀한 정량분석을 하였다. 돼지고기 시료중의 클로람페니콜은 에틸아세테이트로 추출하였으며, 회수율을 높이기 위하여 고체상 추출법(Solid Phase Extraction)을 이용하였다. 액체크로마토그래피/질량분석기는 전기 분무 이온화 장치(Electrospray Ionization, ESI)를 장착하여 음이 온 모드로 선택반응분석법(Selected Reaction Monitoring mode)에서 수행하였다. 클로람페니콜의 분자이온 $[M-H]^-$이온이 조각이온인 $[M-H-(HCOCl)]^-$로 가는 m/z 321 ${\rightarrow}$ 257와 동위원소의 m/z 326 ${\rightarrow}$ 262 채널을 선택하여 분석하였다. 클로람페니콜을 약 0.2, 1, 10, $25\;{\mu}g$/kg의 농도가 되도록 첨가한 돼지고기 시료로부터 제조값과 측정 분석값을 비교하여 검토한 결과, 측정값들은 불확도 범위 내에서 제조값과 일치함을 보였다. 또한 IRMM(Institute for Reference Materials and Measurement)의 클로람페니콜 분석용 돼지고기 시료인 인증 표준물질 BCR 445를 분석한 결과, 본 실험의 측정값은 불확도 범위 내에서 인증값과 일치함을 보였으며 불확도의 경우에는 IRMM이 제공한 값보다 훨씬 향상된 값을 보였다.

Load-Displacement Formulations of Low-rise Unbounded RC Shear Walls with or without Openings

  • Lou, K. Y.;Cheng, F. Y.;Sheu, M. S.;Zhang, X. Z.
    • Computational Structural Engineering : An International Journal
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    • 제1권2호
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    • pp.117-130
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    • 2001
  • Investigations of low-rice unbounded reinforced concrete shear walls with or without openings are performed with comparison of analytical and experimental results. Theoretical analysis is based on nonlinear finite element algorithm, which incorporates concrete failure criterion and nonlinear constitutive relationships. Studios focus on the effects of height-to-length ratio of shear walls, opening ratio, horizontal and vertical reinforcement radios, and diagonal reinforcement. Analytical solutions conform well with experimental results. Equations for cracking, yielding and ultimate loads with corresponding lateral displacements are derived by regression using analytical results and experimental data. Also, failure modes of low-rise unbounded shear walls are theoretically investigated. An explanation of change in failure mode is ascertained by comparing analytical results and ACI code equations. Shear-flexural failure can be obtained with additional flexural reinforcement to increase a wall's capacity. This concept leads to a design method of reducing flexural reinforcement in low-rise bounded solid shear wall's. Avoidance of shear failure as well as less reinforcement congestion leer these walls is expected.

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Repairability Performance and Restoring Force Characteristics of Damaged H-shaped Steel Members after Repair

  • Mori, Kenjiro;Ito, Takumi;Sato, Hanako;Munemura, Hiroka;Matsumoto, Takeshi;Choi, Changhoon
    • 국제초고층학회논문집
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    • 제4권1호
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    • pp.57-64
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    • 2015
  • Recently, new keywords such as "Resilience" and "Repairability" have been discussed from the perspective of the sustainability of damaged structures after a severe disaster. To evaluate the repairability and recovery of structures, it is necessary to establish an analytical method that can simulate the behavior of repaired structures. Furthermore, it is desirable to establish an evaluation method for the structural performance of repaired structures. This study investigates the repairability and recovery of steel members that are damaged by local buckling or cracks. This paper suggests a simple analytical model for repaired steel members, in order to simulate the inelastic behavior and evaluate the recoverability of the structural performance. There is good agreement between the analytical results and the test results. The proposed analytical method and model can effectively evaluate the recoverability.

스펙트럴요소법을 이용한 동적분포하중을 받는 구조물의 동적해석 (Dynamic Analysis of the Structures under Dynamic Distributed Loads Using Spectral Element Method)

  • 이우식;이준근
    • 대한기계학회논문집A
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    • 제20권6호
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    • pp.1773-1783
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    • 1996
  • Finite element method(FEM) is one of the most popularly used method analyzing the dynamic behaviors of structures. But unless number of finite elements is large enough, the results from FEM some what different from exact analytical solutions, especially at high frequency range. On the other hand, as the spectral analysis method(SAM) deals directly with the governing equations of a structure, the results from this melthod cannot but be exact regardless of any frequency range. However, the SAM can be applied only to the case where a structure is subjected to the concentrated loads, despite a structure could be unddergone distributed loads more generally. In this paper, therefore, new spectral analysis algorithm is introduced through the spectral element method(SEM), so that it can be applied to anlystructures whether they are subjected to the concentrated loads or to the distributed loads. The results from this new SEM are compared with both the results from FEM and the exact analytical solutions. As expected, the results from new SEM algorithm are found to be almost identical to the exact analytical solutions while those from FEM are not agreed well with the exact analytical solutions as the mode number increases.

HPLC-MS에 의한 Tri-Octyl Amine(TOA)의 방사선 분해산물 정량 (Determination of radiolysis products in Tri-Octyl Amine by high performance liquid chromatography-mass spectrometer)

  • 양한범;이일희;문형실
    • 분석과학
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    • 제18권3호
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    • pp.201-205
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    • 2005
  • TOA의 방사선 분해산물중 TOA, DOA 및 MOA 함량을 액체크로마토그래피-질량분석기로 정량 분석하였다. Phenomenex LUNA-$C_{18}$ 분리관에서 $CH_3OH$$H_2O$(50 mmol $CH_3COONH_4$) 혼합용액을 이동상으로 하여 TOA, DOA 및 MOA의 머무름 거동을 살펴보았으며, 이동상의 부피비가 85 : 15일 때 방사선 분해산물의 분리가 가장 효율적이었다. MOA, DOA 및 TOA의 분리봉우리는 각각 2.7분, 4.3분, 그리고 16.6분에서 나타났으며, 측정 농도범위는 $30{\sim}160{\mu}g/mL$가 적합하였다. 이 범위에서 검량곡선은 $r2=0.999$의 좋은 상관관계를 보여주었으며, 시료량 $20{\mu}L$를 취할 경우에 SCAN mode에서 TOA, DOA 의 검출한계는 각각 $0.1{\mu}g/mL$, $1{\mu}g/mL$이었고, SIM mode에서 MOA의 검출한계는 $0.1{\mu}g/mL$이었다.

자동핵종분리장치를 이용한 액체시료 중 89Sr, 90Sr 동시분석법 연구 (Simultaneous analysis method of 89Sr and 90Sr in liquid sample using automated separation system)

  • 김희원;이용진;김선하;이진홍;임종명;김현철
    • 분석과학
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    • 제33권6호
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    • pp.274-284
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    • 2020
  • 액체시료 중 89Sr와 90Sr을 자동핵종분리장치를 이용하여 Sr-resin으로 분리-정제하고, 액체섬광계수기(LSC)로 동시 분석하는 방법을 연구하였다. 액체시료 0.5 kg 중 방사성스트론튬을 탄산염 형태로 농축하고, Sr-resin 2 mL (Bed volume)으로 분리하였다. 유량이 최대 1 mL min-1까지 가능한 중력법과, 유량 2 mL min-1, 4 mL min-1 조건에서, Sr과 방해이온들의 거동을 평가하였다. LSC를 이용해 섬광용액을 혼합하지 않은 Cerenkov mode와, 섬광용액을 혼합한 Scintillation mode에서 측정한 결과를 이용해 정제된 89Sr와 90Sr의 방사능을 동시에 분석하였다. 표준선원을 이용해 90Sr/89Sr의 방사능 비가 1:1, 1:2, 1:5 되도록 탈염수를 이용해 모의시료를 준비하였고, 89Sr 방사능은 0.5~10 Bq kg-1, 90Sr 방사능은 0.5~50 Bq kg-1의 범위이다. Sr의 회수율은 68~94 %이고, 89Sr의 상대편의는 -5~20 %, 90Sr 방사능의 상대편의는 -10~10 %로 나타났다.

Simple and Robust Measurement of Blood Plasma Lysophospholipids Using Liquid Chromatography Mass Spectrometry

  • Ji, Dong Yoon;Lee, Chang-Wan;Park, Se Hee;Lee, Eun Jig;Lee, Do Yup
    • Mass Spectrometry Letters
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    • 제8권4호
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    • pp.109-113
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    • 2017
  • Single analytical procedure including extraction, liquid chromatography, and mass spectrometric analysis was evaluated for the simultaneous measurement of lysophospholipids (LPLs). LPLs, particularly, lysophosphatidic acids (LPA) and sphingosine 1-phosphate (S1P) are lipid messengers ubiquitously found in various biological matrix. The molecular species mediate important physiological roles in association with many diseases (e.g. cancer, inflammation, and neurodegenerative disease), which emphasize the significance of the simple and reliable analytical method for biomarker discovery and molecular mechanistic understanding. Thus, we developed analytical method mainly focusing on, but not limited by those lipid species S1P and LPA using reverse phase liquid chromatography-tandem mass spectrometry (RPLC-ESI-MS-MS). Extraction method was modified based on Folch method with optimally minimal level of ionization additive (ammonium formate 10 mM and formic acid). Reverse-phase liquid-chromatography was applied for chromatographical separation in combination with negative ionization mode electrospray-coupled Orbitrap mass spectrometry. The method validation was performed on human blood plasma in a non-targeted lipid profiling manner with full-scan MS mode and data-dependent MS/MS. The proposed method presented good inter-assay precision for primary targets, S1P and LPA. Subsequent analysis of other types of LPLs identified a broad range of lysophosphatidylcholines (LPCs) and lysophosphatidyl-ethanolamines (LPEs).

네트워크 관리 시스템의 해석적 모델 및 성능 평가 (Analytical Models and Performance Evaluations of Network Management Systems)

  • Jung Woo, Lee;Jae Hyuk, Choi;Woo Seok, Lee;Sang Bang, Choi
    • 대한전자공학회논문지TC
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    • 제41권9호
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    • pp.17-28
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    • 2004
  • 인터넷이 급속히 발전하여 통신 하부구조가 됨에 따라 네트워크의 많은 구성요소를 체계적으로 관리하는 네트워크 관리 시스템은 인터넷의 필수 요소가 되고 있다. 네트워크 규모의 급속한 성장은 기존의 SNMP(Simple Network Management Protocol), CMIP(Common Management Information Protocol) 등을 기반으로 한 클라이언트-서버(client-server) 관리 패러다임으로는 한계를 가진다. 따라서 네트워크를 효율적으로 관리하기 위해서 분산형(distributed) 패러다임인 이동에이전트(Mobile Agent)를 네트워크 관리에 이용하려는 연구가 최근에 많이 이루어지고 있다. 본 논문에서는 중앙 집중형의 SNMP, 분산형의 이동에이전트, 그리고 이들 두 접근 방법의 단점을 극복하기 위한 이동에이전트의 한 형태인 혼합모드의 해석적 모델을 제안하고 그 성능을 비교 분석한다 제안한 해석적 모델을 네트워크 응답 시간에 중점을 두어 성능 평가 한 결과 LAN에서는 대체적으로 SNMP가 유리한 반면 WAN에서는 네트워크 환경에 따라 이동에이전트 또는 혼합모드가 더 좋은 응답 시간을 보임을 알 수 있다.

소각시설 소각재의 잔류성 유기오염 물질 분포특성 (The distribution characteristics of persistent organic pollutants in incineration residues at solid waste incinerators)

  • 김종향;이방희;백성복;이인아;이상희;박경호;김현
    • 분석과학
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    • 제22권2호
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    • pp.119-127
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    • 2009
  • 폐기물공정시험법과 내분비계 장애물질 시험방법을 이용하여 사업장폐기물소각재 24건 및 생활 쓰레기소각재 20건에 대하여 잔류성 유기오염물질의 분포특성을 확인하였다. 12종류의 잔류성 유기오염 물질중에서 7종을 GC-MSD (SIM-mode)로 정량분석을 하였다. 총 44건의 시료 중 21 시료에서 헥사클로로벤젠이 검출되었으며, 나머지는 모두 불검출이었다. 헥사클로로벤젠은 사업장폐기물의 소각재에서는 0.132-8.138 ng/g, 비산재에서는 0.195-5.765 ng/g, 그리고 생활쓰레기 소각장의 소각재에서는 0.270-1.828 ng/g, 비산재에서는 0.154-50.643 ng/g 정도로 각각 검출되었다.

The Analysis of Sulfur Compounds of Odorous Material in Kunsan Industrial Complex

  • Kim, Seong-Cheon;Kim, Ki-Hyun;Choi, Yeo-Jin
    • 한국환경보건학회:학술대회논문집
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    • 한국환경보건학회 2005년도 국제학술대회
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    • pp.399-405
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    • 2005
  • In this study, we investigated the gas chromatography (GC) and pulsed flame photometric detection (PFPD) system for the analysis of four major reduced S compounds including hydrogen sulfide ($H_2S)$; methyl mercaptan ($CH_3SH$); dimethyl sulfide (DMS); and dimethyl disulfide(DMDS) contained in environmental samples. To analyze these compounds in high concentration range (above ppb level), we developed a high mode analytical setting with the loop-injection system. By contrast, we also established a low mode setting for the analysis of low concentration samples (ppt-level samples from ambient air) by the combination with thermal desorption unit(TDU). Comparative analysis of both settings revealed that relative detection properties of four S compounds are systematic enough. The results of high mode analysis indicated that the patterns were systematic among compounds: H2S exhibited the lowest sensitivity, while DMBS showed the strongest one. The results were also compared in terms of sensitivity reductions for all compounds by dividing slope ratios between low and high mode system. Although low mode system exhibited significant reductions on the order of a few tens times, their detection characteristics were highly consistent as it was shown in the high mode setting. To learn more about absolute and relative relations between two different modes of S analysis, future studies may have to be directed to cover more complicated nature of GC/PFPD performance. Hydrogen sulfide($H_2S$) was over in summer about low level of olfactory sense 410 ppt, Methyl mercaptan(C$H_3SH$) was over in apring and summer about low level of olfactory sense 70, Dimethyl sulfide(DMS) was not over in four season about low level of olfactory sense 2,200 ppt. Carbon disulfide($CS_2$) was not over in four deason about Tow level of olfactory sense 210,000, Dimethyl disulfide(DMDS) was not over in summer about low level of olfactory sense2,000.

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