• 제목/요약/키워드: standard analytical method

검색결과 903건 처리시간 0.031초

Development of Sensitive Analytical Method of Rhodanthpyrone A by a LC-MS/MS and its Application to Bioavailability Study in Rats

  • Kang, Bitna;Yoon, Jeong A;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • 제10권3호
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    • pp.88-92
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    • 2019
  • A sensitive analytical method of rhodanthpyrone A in rat plasma was developed using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Rhodanthpyrone A and rhodanthpyrone B (internal standard) in rat plasma were extracted by a liquid-liquid extraction method with ethyl acetate. This extraction method gave results in high and reproducible extraction recovery in the range of 73.75-79.90% with no interfering peaks around the peak elution time of rhodanthpyrone A and B. The standard calibration curves for rhodanthpyrone A ranged from 0.5 to 2000 ng/mL were linear with $r^2$ > 0.994 and the inter- and intra-day accuracy and precision and the stability were within acceptance criteria. Using this validated analytical method, pharmacokinetics of rhodanthpyrone A following intravenous and oral administration of rhodanthpyrone A at doses of 2 mg/kg and 30 mg/kg, respectively, were investigated. Rhodanthpyrone A in rat plasma showed multi-exponential elimination pattern with high clearance and volume of distribution values. The absolute oral bioavailability of this compound was calculated as 3.7%. Collectively, the newly developed sensitive LC-MS/MS analytical method of rhodanthpyrone A could be successfully applied to investigate the pharmacokinetic properties of this compound and would be useful for the further studies on the efficacy, toxicity, and biopharmaceutics of rhodanthpyrone A.

석면 분석방법에 대한 고찰 (Review on asbestos analysis)

  • 함승헌;황성호;윤충식;박동욱
    • 한국산업보건학회지
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    • 제19권3호
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    • pp.213-232
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    • 2009
  • This document was prepared to review and summarize the analytical methods for airborne and bulk asbestos. Basic principles, shortcomings and advantages for asbestos analytical instruments using phase contrast microscopy(PCM), polarized light microscopy(PLM), X-ray diffractometer (XRD), transmission electron microscopy(TEM), scanning electron microscopy(SEM) were reviewed. Both PCM and PLM are principal instrument for airborne and bulk asbestos analysis, respectively. If needed, analytical electron microscopy is employed to confirm asbestos identification. PCM is used originally for workplace airborne asbestos fiber and its application has been expanded to measure airborne fiber. Shortcoming of PCM is that it cannot differentiate true asbestos from non asbestos fiber form and its low resolution limit ($0.2{\sim}0.25{\mu}m$). The measurement of airborne asbestos fiber can be performed by EPA's Asbestos Hazard Emergency Response Act (AHERA) method, World Health Organization (WHO) method, International Standard Organization (ISO) 10312 method, Japan's Environmental Asbestos Monitoring method, and Standard method of Indoor Air Quality of Korea. The measurement of airborne asbestos fiber in workplace can be performed by National Institute for Occupational Safety and Health (NIOSH) 7400 method, NIOSH 7402 method, Occupational Safety and Health Administration (OSHA) ID-160 method, UK's Health and Safety Executive(HSE) Methods for the determination of hazardous substances (MDHS) 39/4 method and Korea Occupational Safety and Health Agency (KOSHA) CODE-A-1-2004 method of Korea. To analyze the bulk asbestos, stereo microscope (SM) and PLM is required by EPA -600/R-93/116 method. Most bulk asbestos can be identified by SM and PLM but one limitation of PLM is that it can not see very thin fiber (i.e., < $0.25{\mu}m$). Bulk asbestos analytical methods, including EPA-600/M4-82-020, EPA-600/R-93/116, OSHA ID-191, Laboratory approval program of New York were reviewed. Also, analytical methods for asbestos in soil, dust, water were briefly discussed. Analytical electron microscope, a transmission electron microscope equipped with selected area electron diffraction (SAED) and energy dispersive X-ray analyser(EDXA), has been known to be better to identify asbestiform than scanning electron microscope(SEM). Though there is no standard SEM procedures, SEM is known to be more suitable to analyze long, thin fiber and more cost-effective. Field emission scanning electron microscope (FE-SEM) imaging protocol was developed to identify asbestos fiber. Although many asbestos analytical methods are available, there is no method that can be applied to all type of samples. In order to detect asbestos with confidence, all advantages and disadvantages of each instrument and method for given sample should be considered.

Analysis of Symmetric and Periodic Open Boundary Problem by Coupling of FEM and Fourier Series

  • Kim, Young Sun
    • Journal of Magnetics
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    • 제18권2호
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    • pp.130-134
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    • 2013
  • Most electrical machines like motor, generator and transformer are symmetric in terms of magnetic field distribution and mechanical structure. In order to analyze these problems effectively, many coupling techniques have been introduced. This paper deals with a coupling scheme for open boundary problem of symmetric and periodic structure. It couples an analytical solution of Fourier series expansion with the standard finite element method. The analytical solution is derived for the magnetic field in the outside of the boundary, and the finite element method is for the magnetic field in the inside with source current and magnetic materials. The main advantage of the proposed method is that it retains sparsity and symmetry of system matrix like the standard FEM and it can also be easily applied to symmetric and periodic problems. Also, unknowns of finite elements at the boundary are coupled with Fourier series coefficients. The boundary conditions are used to derive a coupled system equation expressed in matrix form. The proposed algorithm is validated using a test model of a bush bar for the power supply. And the each result is compared with analytical solution respectively.

강박스 거더교 콘크리트 바닥판에 발생하는 크리프, 건조수축, 수화열에 관한 연구 (A Study on Creep, Drying Shrinkage, Hydration Heat Produced in Concrete Floor Plate of Steel Box Girdler Bridge)

  • 강성후;박선준;김민성
    • 한국콘크리트학회:학술대회논문집
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    • 한국콘크리트학회 2003년도 봄 학술발표회 논문집
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    • pp.457-462
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    • 2003
  • It studies the non-structural crack factors that are produced in Steel Box Girder Bridge concrete floor plate using analytical method. It mainly studies humidity and design standard of concrete strength. It used MIDAS CIVIL Ver 5.4.0, a general structure analysis program that applies drying shrinkage rate of domestic road bridge design standard and standard value of creep coefficient, CEF-FIP standard equation and ACI standard equation from the aspect of creep, drying shrinkage and hydration heat to see the effect of the two factors on concrete crack and found the following result. The analytical results of this study showed that the initial stress, which was obtained by ACI standard, exceeds the allowable tensile stress between 5 to 18 days. This result means that even if a bridge is designed and constructed according to design standard, the bridge can have cracks due to various variables such as drying shrinkage, hydration heat and creep that produce stress in slab.

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의약품 함량분석 정도관리에서의 변이 요인에 대한 통계분석 (Statistical Analysis on the Sources of Variance in Proficiency Test of Quantitative Analysis of Medicines)

  • 조정환
    • Journal of Pharmaceutical Investigation
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    • 제37권1호
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    • pp.27-37
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    • 2007
  • Proficiency test is an essential tool far ensuring analytical ability of analytical chemists and analytical institutes. Usually, the standard protocol for proficiency test is focused on acceptability of reported analytical results of participants by calculating z-scores and related diagnostic parameters. The ultimate goal of this process is to reveal the sources of variability of analytical results and to find the way to reduce their influence. In this study, the method of analysis of variance (ANOVA) was applied to the analytical data collected from qualify control departments of pharmaceutical companies in KyungIn province in Korea in the year of 2000. As influencing factors of variability of analytical results, the use of internal standards for liquid and gas chromatograpy, the educational and professional background of participants, geological locations and yearly production sizes of participating companies were evaluated. To evaluate the variability in accuracy of analytical results, absolute differences from sample mean and sample median were used and to evaluate variability in precision of individual participants, the reported standard deviation of each participant was used. As a result, the use of internal standards in gas chromatographic analysis, participants' academic background and the yearly production sizes of pharmaceutical companies showed statistically significant influence to the accuracy and the precision of the reported analytical results used in this study.

다중 모세관을 이용한 교정용 표준가스의 제조: 불확도와 유효성 평가 (Generation of calibration standard gases using capillary gas divider: uncertainty measurement and method validation)

  • 이상윤;황은진;정혜자;이광우;전기준
    • 분석과학
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    • 제19권5호
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    • pp.369-375
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    • 2006
  • ISO 6145-5에 의거한 동적 부피 측정법을 이용하여 교정용 혼합가스를 제조하고 그 불확도를 평가하였다. 내경 0.25 mm, 길이 50 cm 규격의 10개의 모세관을 병렬 배치하고, 성분 가스와 희석 가스가 흐르는 모세관 개수를 조절하는 방법으로 혼합 가스의 희석 비율을 결정하였다. 모세관은 각종 가스에 대하여 낮은 흡착 용량을 가진 PTFE 재질의 것을 사용하였으며, 유로의 설정은 열을 발생시키지 않는 mechanical valve를 사용하였다. ISO 6145-5의 요건을 구현하는 본 장치를 이용하여 제조된 희석 가스의 농도는 (주)리가스에서 제조한 마스터급 표준가스를 이용하여 비교 평가하였다. ISO 6143의 비교법을 이용한 교정 후 제조된 산소 표준가스의 농도 편차는 대부분의 희석 영역에서 상대비 0.2% 이내, 황화수소 표준가스의 농도 편차는 상대비 1% 이내임을 확인하였다. 이 결과는 본 장치를 통해 제조한 표준가스가 대기환경 측정용 등 저농도 표준가스를 이용한 교정 곡선 획득용으로 사용하는데 충분한 성능을 가지고 있음을 증명하는 것이다.

Development Rapid Analytical Methods for Inositol as a Trace Component by HPLC and LC-MS/MS in Infant Formula

  • Shin, Jin-Ho;Park, Jung-Min;Kim, Ha-Jung;Ahn, Jang-Hyuk;Kwak, Byung-Man;Kim, Jin-Man
    • 한국축산식품학회지
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    • 제35권4호
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    • pp.466-472
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    • 2015
  • A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor.

Response determination of a viscoelastic Timoshenko beam subjected to moving load using analytical and numerical methods

  • Tehrani, Mohammad;Eipakchi, H.R.
    • Structural Engineering and Mechanics
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    • 제44권1호
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    • pp.1-13
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    • 2012
  • In this paper the dynamic behavior of a viscoelastic Timoshenko beam subjected to a concentrated moving load are studied analytically and numerically. The viscoelastic properties of the beam obey the linear standard model in shear and incompressible in bulk. The governing equation for Timoshenko beam theory is obtained in viscoelastic form using the correspondence principle. The analytical solution is based on the Fourier series and the numerical solution is performed with finite element method. The effects of the material properties and the load velocity are investigated on the responses by numerical and analytical methods. In addition, the results are compared with the Euler beam results.

대체용매를 이용한 금속가공유 측정방법 타당성 평가 (Validation of an Extraction Method for the Determination of Airborne MWFs using Alternative Solvents)

  • 정지연;백남원
    • 한국산업보건학회지
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    • 제16권2호
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    • pp.91-100
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    • 2006
  • The purpose of this study was to validate alternative method by using non-carcinogenic, and less toxic solvents than NIOSH analytical method 5524 for measuring the airborne MWFs in workplaces. In laboratory tests, the ETM solvents(mixture of same volume for ethyl ether, toluene, and ethanol) were selected. The alternative method of analyzing MWFs, referred to as the ETM solvent extraction method, showed 0.04 mg/sample as LOD, and 0.15 mg/sample as LOQ. The analytical precision (pooled CV, coefficient of variation) of the ETM solvent extraction method for analyzing the straight, soluble, semisynthetic, and synthetic metalworking fluid was 1.5%, 2.0%, 2.6%, 1.6%, respectively, which was similar to the precision (2.6%) of NIOSH analytical method (NIOSH 0500) for total dust. The analytical accuracy by recovery test, spiked mass calculated as extractable mass, was almost 100%. As the result of storage stability test, metalworking fluid samples should be stored in refrigerated condition, and be analyzed in two weeks after sampling. The 95% confidence limit of the estimated total standard error for the ETM solvent extraction method for analyzing the straight, soluble, semisynthetic, and synthetic metalworking fluid was ${\pm}12.6%$, ${\pm}12.5%$, ${\pm}14.0%$, and ${\pm}13.6%$, respectively, which satisfied the OSHA sampling and analytical criteria.