• 제목/요약/키워드: 3-D Analytical Method

검색결과 482건 처리시간 0.029초

알칼리분해를 이용한 어류 중 다환방향족탄화수소의 전처리방법 (Pretreatment of Fish for the determination of polycyclic aromatic hydrocarbons using alkali digestion)

  • 허수정;이효민;채영주;유은아
    • 분석과학
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    • 제18권5호
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    • pp.403-409
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    • 2005
  • 최근 내분비계장애물질로 알려진 PAHs 화합물 중 하나인 벤조피렌은 대표적인 PAHs 화합물로 음식을 조리, 가공할 때 식품의 주성분인 탄수화물, 단백질, 지방 등이 분해되어 생성되는 열분해 산물이며 토양, 공기, 물, 식품 등 전 환경매체에서 검출되고 있다. 본 연구에서는 PAHs[benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno(1,2,3-c,d)pyrene]에 대하여 어류 중 지방의 알칼리 분해시간에 따른 분해효율, 추출 용매에 따른 추출효율, 정제컬럼의 용출량에 따른 정제효율 등을 비교 실험하여 알칼리분해를 이용한 어류 중 PAHs의 전처리방법을 확립하고자 하였다. 균질화된 시료를 알칼리 분해하여 n-hexane으로 추출하고 증류수로 세척한 후 Sep-Pak florisil cartridge로 정제하여 HPLC/FLD(고속액체크로마토그래피/형광검출기) 로 동시 정량 분석하였으며 각각의 PAHs에 대한 회수율은 약 90~106% 수준이었다.

두릅 추출물의 기능성 원료 표준화를 위한 HPLC 분석법 검증 (HPLC analytical method validation of Aralia elata extract as a functional ingredients)

  • 안은미;최송암;최지영
    • 한국식품저장유통학회지
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    • 제24권6호
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    • pp.795-801
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    • 2017
  • 개별인정형 건강기능식품 기능성 원료로 개발한 두릅추출물의 표준화를 위해 항고혈압활성 효과를 가지고 있는 기능성분 HE를 지표성분으로 설정하고, HPLC/UV 방법을 이용하여 기능성분 분석법을 확립하며 그에 따른 유효성 검증을 실시하고자 하였다. 유효성 검증 결과, 본 시험법에서 표준용액의 피크유지시간과 두릅추출물의 피크유지시간이 일치하였다. 검량선의 결정 계수(R2)는 0.9999 이상의 높은 직선성을 보여 분석에 적합함을 알 수 있었으며, 검출 한계는 $12.0{\mu}g/mL$, 정량한계는 $36.5{\mu}g/mL$로 두릅 추출물 중의 HE 함량분석을 위한 충분한 한계 수준으로 확인되었다. 정확성에서 $98.8{\pm}0.865-104.7{\pm}2.536%$로 높은 수준의 HE 회수율을 보였으며, 평균 분석오차는 0.013%로서 기준인 10% 이내를 만족하였다. 또한 반복성에서는 평균 $101.5{\pm}0.4%$로 RSD 0.4%를 나타내었고, 실험실내 정밀성에서 RSD 0.2%, 완건성에서 RSD 0.2%를 나타내어 모두 적합함을 확인하였다. 한편, 제주산 두릅추출물 중에는 기능성 지표성분인 HE가 4.88% 함유되어 있는 것으로 확인되었다. 이상의 실험 결과, 두릅추출물의 항고혈압활성 기능성분인 HE의 HPLC/UV 분석방법은 특이성, 직선성, 정확성, 정밀성, 반복성, 완건성 등의 모든 항목에서 validation 기준에 적합한 시험 방법으로 확인되었다.

Analysis and Modeling of Magnetic Characteristics in Surface-Mounted Permanent-Magnet Machines with Rotor Overhang

  • Yeo, Han-Kyeol;Woo, Dong-Kyun;Lim, Dong-Kuk;Ro, Jong-Suk;Jung, Hyun-Kyo
    • Journal of international Conference on Electrical Machines and Systems
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    • 제2권4호
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    • pp.399-404
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    • 2013
  • The rotor overhang is used to enhance air-gap flux and improve power density. Due to asymmetry in the axial direction caused by the overhang, the time consuming 3D analysis is necessary to design the motor with overhang. To solve this problem, this paper proposes the equivalent magnetic circuit model (EMCM) that can consider overhang effects without the 3D analysis by using effective air-gap length. The analysis time can be reduced significantly via the proposed EMCM. The reduction of the analysis time is essential for the preliminary design of the motor. In order to verify the proposed model, the 3-D finite-element method (FEM) analysis is adopted. 3-D FEM results confirm the validity of the proposed EMCM.

Sulfurous acid 환원제를 이용한 ICP-AES에 의한 Osmium의 정량 분석 (Determination of osmium using sulfurous acid as reductant by ICP-AES)

  • 박한석;김강진
    • 분석과학
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    • 제20권3호
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    • pp.251-254
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    • 2007
  • 수용액 내에서 환원제인 sulfurous acid와 휘발성이 강한 Os(III)을 반응시킨 후 생성된 비휘발성 Os(IV)을 inductively coupled plasma atomic emission spectrometry (ICP-AES)로 분석하였다. pH 2-10의 수용액에서 sulfurous acid와 Os(VIII)의 정량적 반응에 의하여 생성된 Os(VI)을 ICP-AES로 분석하였다. 동축형 분무기(concentric type nebulizer)에 의한 시료 도입 방법에서 sulfurous acid와 osmium은 반응 직후부터 안정한 신호를 나타내었으며 다양한 ICP-AES 조건에서 3회 반복 측정했을 때 재현성은 0.5-4.5%였으며, 검출 한계는 2.5-57.7 ng/g이었다.

Qualitative and quantitative assessment of process related impurities in Brigatinib raw material and formulations using HPLC

  • Attada Tharun;Potnuru Jagadeesh;B Srinivasa Kumar;Kota Thirumala Prasad;Venkateswara Rao Anna
    • 분석과학
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    • 제36권4호
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    • pp.180-190
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    • 2023
  • The presence of process related impurities in any drug or the drug product was associated with its safety, stability and efficacy. The overall literature survey proved that there is no method published on the assessment of process related impurities in brigatinib. In this study, a simple, reliable and stable HPLC qualitative method was reported for quantification of process related impurities with easy and quick extraction procedure. The impurities along with standard brigatinib was resolved on Lichrospher® C18 (250 mm × 4.6 mm; 5 ㎛ particle size) column in room temperature using methanol, acetonitrile, pH 4.5 phosphate buffer in 55:25:20 (v/v) at 1.0 mL/min as mobile phase and UV detection at 261 nm. The method produces well resolved peaks at retention time of 4.60 min, 12.28 min, 3.37 min, 7.34 min and 8.39 min respectively for brigatinib, impurity A, B, C and D. The method produces a very sensitive detection limit of 0.0065 ㎍/mL, 0.0068 ㎍/mL, 0.0053 ㎍/mL and 0.0058 ㎍/mL for impurity A, B, C and D respectively with calibration curve linear in the concentration range of 22.5-135 ㎍/mL for brigatinib and 0.0225-0.135 ㎍/mL for impurities. The method produces all the validation parameters under the acceptable level and doesn't produces any considerable changes in peak area response while minor changes in the developed method conditions. The method can effectively resolve the unknown stress degradation products along with known impurities with less % degradation. The method can efficiently resolve and quantify the impurities in formulation and hence can suitable for the routine quality analysis of brigatinib in raw material and formulation.

균열암반의 역학적 등가물성의 수치해석적 결정을 위한 2차원 및 3차원 해석의 비교 (Comparison of Two- and Three-dimensional Approaches for the Numerical Determination of Equivalent Mechanical Properties of Fractured Rock Masses)

  • 민기복;알렌토로발
    • 터널과지하공간
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    • 제22권2호
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    • pp.93-105
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    • 2012
  • 균열암반의 등가역학적 물성을 수치해석적으로 결정할 때 2차원 및 3차원 해석을 비교하였다. 수직균열모델과 암반균열망(DFN) 모델이 균열암반의 형상으로 이용되었으며 3차원 모델으로부터 다양한 방향으로 2차원 모델을 절단하여 역학적 물성을 비교하였다. 본 연구의 지질데이터는 영국 셀라필드 지역의 자료를 기본으로 사용하였다. 직교균열모델에서는 컴플라이언스텐서의 변환을 이용한 해석적 방법이 물성결정을 위해 이용되었으며 암반균열망모델에서는 수치실험이 실시되었다. 2차원 모델에서는 균열이 항상 모델평면과 직교한다고 가정하기 때문에 탄성계수는 항상 3차원보다 크게 계산이 되었다. 2차원 해석에서의 포아송비는 3차원 해석보다 큰 값을 나타내는 경향이 있었으나 반대의 경향도 관찰되었다. 본 논문은 3차원 형상을 단순화시켜 사용하는 2차원 해석의 한계를 정량적으로 고찰하였다는데 의의가 있다.

QuEChERS법을 활용한 농산물 중 제초제 Tolpyralate의 최적 분석법 선발 및 검증 (Application and Validation of an Optimal Analytical Method using QuEChERS for the determination of Tolpyralate in Agricultural Products)

  • 이한솔;박지수;이수정;신혜선;김지영;윤상순;정용현;오재호
    • 한국환경농학회지
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    • 제39권3호
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    • pp.246-252
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    • 2020
  • BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R2≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.

Numerical Investigation of an Unconditionally Stable Compact 2D FDTD Based on the Alternating-Direction Implicit Scheme

  • Saehoon Ju;Jeongnam Cheon;Kim, Hyung-Hoon;Kim, Hyeongdong
    • Journal of electromagnetic engineering and science
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    • 제3권1호
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    • pp.39-44
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    • 2003
  • An unconditionally stable compact 2D Alternating-Direction Implicit (ADI) FDTD method for calculating dispersion characteristics of waveguide structures is proposed. The numerical stability and numerical dispersion relation of the proposed method are also presented and discussed. Numerical wavelengths for the dominant and higher order modes in a hollow waveguide are obtained from numerical simulations and compared with those from the analytical dispersion relation. The numerical results show that the proposed scheme has the potential to successfully analyze a class of waveguides having locally fine geometry with reduced numerical costs.

직교 직물 복합재료 물성치 예측을 위한 가상 수치 실험 (Virtual Experimental Characterization of 3D Orthogonal Woven Composite Materials)

  • 이창성;신헌;김승조
    • 한국복합재료학회:학술대회논문집
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    • 한국복합재료학회 2001년도 춘계학술발표대회 논문집
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    • pp.205-210
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    • 2001
  • In this work, virtual material characterization of 3D orthogonal woven composites is performed to predict the elastic properties by a full scale FEA. To model the complex geometry of 3D orthogonal woven composites, an accurate unit structure is first prepared. The unit structure includes warp yarns, filler yarns, stuffer yams and resin regions and reveals the geometrical characteristics. For this virtual experiments by using finite element analysis, parallel multifrontal solver is utilized and the computed elastic properties are compared to available experimental results and the other analytical results. It is founded that a good agreement between material properties obtained from virtual characterization and experimental results. Using the method of this virtual material characterization, the effects of inconsistent filler yarn distribution on the in-plane shear modulus and filler yarn waviness on the transverse Young's modulus are investigated. Especially, the stiffness knockdown of 3D woven composite structures is simulated by virtual characterization. Considering these results, the virtual material characterization of composite materials can be used for designing the 3D complex composite structures and may supplement the actual experiments.

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3D stress-fractional plasticity model for granular soil

  • Song, Shunxiang;Gao, Yufeng;Sun, Yifei
    • Geomechanics and Engineering
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    • 제17권4호
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    • pp.385-392
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    • 2019
  • The present fractional-order plasticity models for granular soil are mainly established under the triaxial compression condition, due to its difficult in analytically solving the fractional differentiation of the third stress invariant, e.g., Lode's angle. To solve this problem, a three dimensional fractional-order elastoplastic model based on the transformed stress method, which does not rely on the analytical solution of the Lode's angle, is proposed. A nonassociated plastic flow rule is derived by conducting the fractional derivative of the yielding function with respect to the stress tensor in the transformed stress space. All the model parameters can be easily determined by using laboratory test. The performance of this 3D model is then verified by simulating multi series of true triaxial test results of rockfill.