• Title/Summary/Keyword: Analytical Validation

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Development and Validation of the Simultaneous Analytical Method of Urinary Metals and Metalloids for the National Biomonitoring Programs (국가 바이오모니터링 프로그램을 위한 소변 중 금속류 동시분석법 개발 및 검증)

  • Cho, Yong Min;Yang, Minho;Im, Hosub;Cha, Sangwon;Lee, Jaeick;Kim, Ki Hun;Han, Sang Beom
    • Journal of Environmental Health Sciences
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    • v.45 no.6
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    • pp.594-604
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    • 2019
  • Objectives: This study developed and validated an analysis method of urinary metals and metalloids that can be applied inductively with coupled plasma mass spectrometry (ICP-MS). Methods: 0.3 mL of urine was used to analyze 25 metal and metalloid compounds using ICP-MS. The validation of the analytical method included linearity, accuracy, precision, and the calculation of detection limits. In addition, a comparison test was performed with the graphite furnace atomic absorption spectrometry (GF-AAS) method, which is the current standard method, with urine samples of 66 healthy subjects. Results: The linearities (R2) of calibration curves of all 25 compounds were ≥ 0.999. Of the 25 compounds, the intra-day and inter-day accuracy% of 17 and 20 met ≤15%, respectively. In addition, fifteen compounds showed ≤15% recovery% for certificated reference materials. Intraclass correlation coefficients of the comparison between the current methods and new methods in this study were 0.952 (p-value<0.001) and 0.911 (p-value<0.001) for urinary cadmium and mercury, respectively. Conclusion: This study proposes an efficient simultaneous methodology that can analyze multi elements in smaller sample amounts. More reproduction experiments are needed in the future.

Method Validation and Uncertainty Estimation for Toluene Measurement in Biological Fluids by HS-GC (HS-GC에 의한 생체 시료내 톨루엔 분석에 대한 방법의 유효화와 불확도 추정)

  • Heo, Sangcheol;Min, Ji-Sook;Park, Jongseo;Lim, Mi-Ae;Park, Sungwoo
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.443-453
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    • 2004
  • Toluene is currently used as a major organic solvent of glues which are abused by the youngster for its hallucinogenic effect. In this study, toluene determination method using headspace gas chromatography (HS-GC) in the biological fluids like blood, urine and saliva of glue sniffers was validated and related uncertainties were estimated. LOD of $0.01{\mu}g/mL$ in saliva and LOQ of $0.1{\mu}g/mL$ in blood were the highest among LODs and LOQs in urine, blood and saliva. Other performance characteristics such as linearity, working range, accuracy, precision and recovery were also measured. The uncertainty at toluene concentration of $1{\mu}g/mL$ was estimated to be 0.13, 0.09 and $0.17{\mu}g/mL$ for blood, urine and saliva, respectively, and the uncertainty contribution from the least linear regression was dominant at the lower concentration of toluene.

Validation of a Robust Flutter Prediction by Optimization

  • Chung, Chan-Hoon;Shin, Sang-Joon
    • International Journal of Aeronautical and Space Sciences
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    • v.13 no.1
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    • pp.43-57
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    • 2012
  • In a modern aircraft, there are many variations in its mass, stiffness, and aerodynamic characteristics. Recently, an analytical approach was proposed, and this approach uses the idea of uncertainty to find out the most critical flight flutter boundary due to the variations in such aerodynamic characteristics. An analytical method that has been suggested to predict robust stability is the mu method. We previously analyzed the robust flutter boundary by using the mu method, and in that study, aerodynamic variations in the Mach number, atmospheric density, and flight speed were taken into consideration. The authors' previous attempt and the results are currently quoted as varying Mach number mu analysis. In the author's previous method, when the initial flight conditions were located far from the nominal flutter boundary, conservative predictions were obtained. However, relationships among those aerodynamic parameters were not applied. Thus, the varying Mach number mu analysis results required validation. Using an optimization approach, the varying Mach number mu analysis was found out to be capable of capturing a reasonable robust flutter boundary, i.e., with a low percentage difference from boundaries that were obtained by optimization. Regarding the optimization approach, a discrete nominal flutter boundary is to be obtained in advance, and based on that boundary, an interpolated function was established. Thus, the optimization approach required more computational effort for a larger number of uncertainty variables. And, this produced results similar to those from the mu method which had lower computational complexity. Thus, during the estimation of robust aeroelastic stability, the mu method was regarded as more efficient than the optimization method was. The mu method predicts reasonable results when an initial condition is located near the nominal flutter boundary, but it does not consider the relationships that are among the aerodynamic parameters, and its predictions are not very accurate when the initial condition is located far from the nominal flutter boundary. In order to provide predictions that are more accurate, the relationships among the uncertainties should also be included in the mu method.

Capacity Estimation Models for Work-zones Under Traffic Signal Influence and the Empirical Validation (신호영향권 하 도로공사구간에서의 용량산정모형 개발과 실증)

  • Shin, Chi-Hyun
    • Journal of Korean Society of Transportation
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    • v.31 no.1
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    • pp.77-86
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    • 2013
  • This paper focuses on the development of analytical models for estimating the changes in saturation flow rates (SFR) at the stop-lines of a signalized intersection due to the existence of nearby work-zones, and thereby calculating the prevailing capacity values for specific lane groups. Major changes were incorporated in the logics of previous models and significant revisions have been made to secure the accuracy and simplicity. Furthermore, much attention was paid to model validation by making comparisons to both extensive simulation results and empirical data from various sites. It was found that SFRs are highly sensitive to the location of work-zones, the distance to each work-zone from the stop-line of a concerned approach, the number of lanes open and closed, and the effective green time. Using such geometric and operating conditions that constitute work-zone environment, the proposed models successfully estimated SFR values with a miniscule margin of error.

Development and Validation of Dithiocarbamates Fungicide Analytical Method using CS2 Trap Method in Livestock Product (축산물 중 CS2 포집방법을 이용한 Dithiocarbamate계 살균제 분석법 개발 및 검증)

  • Jo, Hyeong-Wook;Sun, Jung-Hun;Heo, Hyo-Min;Lee, Sang-Hyeob;Kim, Jang-Eok;Moon, Joon-Kwan
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.127-133
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    • 2021
  • BACKGROUND: Dithiocarbamte fungicides have been used in crop cultivation for diseases protection and treatment. And cultivated agricultrual products were used as feedstuff, and residual pesticides are likely to be absorbed and transferred to livestock. But the maximum residue limits (MRLs) were not established for dithiocarbate fungicides in livestock products, and thus an analysis method was developed and validated for dithiocarbamate fungicides to establish MRLs. METHODS AND RESULTS: Samples were prepared using CS2 trap method and detected with UV/VIS spectrophotometer. Calibration line (0.1 ~ 10 ㎍/mL) was linear with r2 > 0.99. For validation, the recovery tests were carried out at three fortification levels (MLOQ, 10 MLOQ and 50 MLOQ) from livestock samples (egg, milk, beef, pork, and chicken). The results for mancozeb, propineb, and thiram ranged between 76.8 to 109.6%, 79.4 to 108.8%, and 80.2 to 107.8%, respectively and % RSD (relative standard deviation) values were below 9.5%. Furthermore, inter-laboratory analysis was performed to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). This might be used as an official analytical method for determination of dithiocarbamate fungicides at established MRLs and monitoring.

Optimization of Extraction Conditions for Swertiamarin in Swertia japonica Makino (당약의 swertiamarin 분석을 위한 추출조건 최적화)

  • Kim, Tae Hee;Jang, Seol;Lee, Ah Reum;Lee, A Young;Choi, Goya;Kim, Ho Kyoung
    • The Korea Journal of Herbology
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    • v.29 no.1
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    • pp.13-18
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    • 2014
  • Objectives : Iridoid glycoside, swertiamarin is a well known bioactive component found in Swertia japonica Makino (SJ). In this study, we tried to optimize a suitable method which would extract swertiamarin effectively. Methods : Extraction of SJ was carried out by various conditions of time (5 - 60 min), temperature ($30-70^{\circ}C$), solvent (from non-polar to polar), and ratio of solvnet / sample (10 : 1 - 40 : 1) using ultrasonic extractor. Swertiamarin in SJ extracts was quantified by high performance liquid chromatography - Phtodiode array detector (HPLC-PDA) using C18 column and the analytical procedure was validated by evaluation of specificity, range, linearity, accuracy (recovery), precision (intra- and inter day variability), limit of detection (LOD), and limit of quantification (LOQ). Results : An efficient extraction condition for swertiamarin in SJ was optimized using sonicator extraction (temperature $40^{\circ}C$, solvent 20% methanol, solvent / sample (20 : 1), and time 10 min. Analytical procedure was optimized by HPLC-PDA using isocratic solvent system of acetonitrile and water (9 : 91), and the method was validated in regard to linearity (correlation coefficient, $R^2$ > 0.9999), range ($50-1000{\mu}g/mL$), intra- and inter-precision (RSD < 5.0 %), and recovery (99 -103 %). LOD and LOQ were 0.051 and $0.155{\mu}g/mL$, respectively. Conclusion : An optimized method of extraction for swertiamarin in SJ was established through conditions of diverse extraction and the validation result indicated that the method is suited for the determination of swertiamarin in SJ.

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
    • Analytical Science and Technology
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    • v.36 no.4
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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.

Validation of the semi-analytical algorithm for estimating vertical underwater visibility using MODIS data in the waters around Korea

  • Kim, Sun-Hwa;Yang, Chan-Su;Ouchi, Kazuo
    • Korean Journal of Remote Sensing
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    • v.29 no.6
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    • pp.601-610
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    • 2013
  • As a standard water clarity variable, the vertical underwater visibility, called Secchi depth, is estimated with ocean color satellite data. In the present study, Moderate Resolvtion Imaging Spectradiometer (MODIS) data are used to measure the Secchi depth which is a useful indicator of ocean transparency for estimating the water quality and productivity. To estimate the Secchi depth $Z_v$, the empirical regression model is developed based on the satellite optical data and in-situ data. In the previous study, a semi-analytical algorithm for estimating $Z_v$ was developed and validated for Case 1 and 2 waters in both coastal and oceanic waters using extensive sets of satellite and in-situ data. The algorithm uses the vertical diffuse attenuation coefficient, $K_d$($m^{-1}$) and the beam attenuation coefficient, c($m^{-1}$) obtained from satellite ocean color data to estimate $Z_v$. In this study, the semi-analytical algorithm is validated using temporal MODIS data and in-situ data over the Yellow, Southern and East Seas including Case 1 and 2 waters. Using total 156 matching data, MODIS $Z_v$ data showed about 3.6m RMSE value and 1.7m bias value. The $Z_v$ values of the East Sea and Southern Sea showed higher RMSE than the Yellow Sea. Although the semi-analytical algorithm used the fixed coupling constant (= 6.0) transformed from Inherent Optical Properties (IOP) and Apparent Optical Properties (AOP) to Secchi depth, various coupling constants are needed for different sea types and water depth for the optimum estimation of $Z_v$.

Analytical method development for residual metamizol in meat using LC/MS/MS (식육 중 메타미졸 잔류물의 LC/MS/MS 시험법 개발)

  • Kim, Tae-Wook;Yang, Yeung-Kyong;Gwoak, Soon-Chul;Kang, Dong-Young
    • Analytical Science and Technology
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    • v.24 no.4
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    • pp.237-242
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    • 2011
  • In this study, an analytical method was developed for residual metamizol in beef and pork using LC/MS/MS. 4-methylaminoantipyrin (MAA), the main metabolite of metamizol was targeted for analysis instead of its parent compound. MAA was simply extracted from meat by acetonitrile, purified and then analyzed by multiple reaction monitoring method (MRM). Standard addition method was used for calibration. The calibration curves showed the linearity of $r^2$ > 0.99 for both matrices included. The developed method was validated by six-time intra-lab tests and inter-lab tests with two other institutes. The validation of the whole procedure for beef showed the intra-lab accuracies of 78-102% (CV 5.5-9.1%) and the inter-lab accuracy of 98% (CV 14%); the intra-lab accuracies of 95-99% (CV 3.9-5.6%) and the inter-lab accuracy of 111% (CV 13%).

POSCA: A computer code for fission product plateout and circulating coolant activities within the primary circuit of a high temperature gas-cooled reactor

  • Tak, Nam-il;Lee, Jeong-Hun;Lee, Sung Nam;Jo, Chang Keun
    • Nuclear Engineering and Technology
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    • v.52 no.9
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    • pp.1974-1982
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    • 2020
  • Numerical prediction of fission product plateout and circulating coolant activities under normal operating conditions is crucial in the design of a high temperature gas-cooled reactor (HTGR). The results are used for the maintenance and repair of the components as well as the safety analysis regarding early source terms under loss of coolant accident scenarios. In this work, a new computer code named POSCA (Plate-Out Surface and Circulating Activities) was developed based on a one-dimensional model to evaluate fission product plateout and circulating coolant activities within the primary circuit of a HTGR. The verification and validation of study for the POSCA code was done using available analytical results and two in-pile experiments (i.e., OGL-1 and VAMPYR-1). The results of the POSCA calculations show that POSCA is able to simulate plateout and circulating coolant activities in a HTGR with fast computation and reasonable accuracy.