• Title/Summary/Keyword: method validation #5

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Selection and Validation of an Analytical Method for Trifludimoxazin in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Trifludimoxazin의 시험법 선정 및 검증)

  • Sun Young Gu;Su Jung Lee;So eun Lee;Chae Young Park;Jung Mi Lee;Inju Park;Yun Mi Chung;Gui Hyun Jang;Guiim Moon
    • Journal of Food Hygiene and Safety
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    • v.38 no.3
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    • pp.79-88
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    • 2023
  • Trifludimoxazin is a triazinone herbicide that inhibits the synthesis of protoporphyrinogen oxidase (PPO). The lack of PPO damages the cell membranes, leading to plant cell death. An official analytical method for the safety management of trifludimoxazin is necessary because it is a newly registered herbicide in Korea. Therefore, this study aimed to develop a residual analysis method to detect trifludimoxazin in five representative agricultural products. The EN method was established as the final extraction method by comparing the recovery test and matrix effect with those of the QuEChERS method. Various sorbent agents were used to establish the clean-up method, and no differences were observed among them. MgSO4 and PSA were selected as the final clean-up conditions. We used LC-MS/MS considering the selectivity and sensitivity of the target pesticide and analyzed the samples in the MRM mode. The recovery test results using the established analysis method and inter-laboratory validation showed a valid range of 73.5-100.7%, with a relative standard deviation and coefficient of variation less than 12.6% and 14.5%, respectively. Therefore, the presence of trifludimoxazin can be analyzed using a modified QuEChERS method, which is widely available in Korea to ensure the safety of residual insecticides.

Method Validation and Quantification of Lutein and Zeaxanthin from Green Leafy Vegetables using the UPLC System (UPLC를 이용한 lutein과 zeaxanthin의 분석법 검증 및 엽채류에서의 정량적 평가)

  • Kim, Suna;Kim, Ji-Sun
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.686-691
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    • 2012
  • The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

Estimation of the Pollutant Removal Efficiency in a Buffer Strip Using a SWAT Model

  • Lee, Eun-Jeong;Choi, Kyoung-Sik;Kim, Tae-Geun
    • Environmental Engineering Research
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    • v.16 no.2
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    • pp.61-67
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    • 2011
  • The water quality from nonpoint source run off results from different land use types has been studied. The construction of a buffer strip is one method of nonpoint source pollutant control. The Soil and Water Assessment Tool (SWAT) model has been applied to estimate the pollutant removal through the buffer strip. When the non-business land has been changed into grass to form a buffer-strip, the change of land use effects the results of the model according to measures of the water quality. The data from a water level station within the watershed in the years 2006 and 2007 was used for calibration and validation of the model. Under the rainfall conditions in 2007, the removal rates of SS, BOD, TN, TP were 11.5%, 9.5%, 1.2%, and 4.5%, respectively. During the rainy days, the removal rates at the buffer strip were 92.3% of SS, 91.2% of BOD, 82.4% of TN, and 83.5% of TP. The pollutants from nonpoint sources were effectively removed by over 80% as they passed through the buffer strips. Rainfall resulted in soil erosion, which led to an increase in the SS concentration, therefore, the construction of buffer strips protected the streams from SS inflows. Since TN concentrations are affected by the inflows of ground water and the N concentration of the rainfall, the removal rate of TN was relatively lower than for the other pollutants.

Discrete element modeling of strip footing on geogrid-reinforced soil

  • Sarfarazi, Vahab;Tabaroei, Abdollah;Asgari, Kaveh
    • Geomechanics and Engineering
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    • v.29 no.4
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    • pp.435-449
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    • 2022
  • In this paper, unreinforced and geogrid-reinforced soil foundations were modeled by discrete element method and this performed under surface strip footing loads. The effects of horizontal position of geogrid, vertical position, thickness, number, confining pressure have been investigated on the footing settlement and propagation of tensile force along the geogrids. Also, interaction between rectangular tunnel and strip footing with and without presence of geogrid layer has been analyzed. Experimental results of the literature were used to validation of relationships between the numerically achieved footing pressure-settlement for foundations of reinforced and unreinforced soil. Models and micro input parameters which used in the numerical modelling of reinforced and unreinforced soil tunnel were similar to parameters which were used in soil foundations. Model dimension was 1000 mm* 600 mm. Normal and shear stiffness of soils were 5*105 and 2.5 *105 N/m, respectively. Normal and shear stiffness of geogrid were 1*109 and 1*109 N/m, respectively. Loading rate was 0.001 mm/sec. Micro input parameters used in numerical simulation gain by try and error. In addition of the quantitative tensile force propagation along the geogrids, the footing settlements were visualized. Due to collaboration of three layers of geogrid reinforcements the bearing capacity of the reinforced soil tunnel was greatly improved. In such practical reinforced soil formations, the qualitative displacement propagations of soil particles in the soil tunnel and the quantitative vertical displacement propagations along the soil layers/geogrids represented the geogrid reinforcing impacts too.

Comparison on Nano-particle Number Measurement Characteristics for Different Particle Generators between Spray type and Soot Type (Spray type과 Soot type 입자발생기별 나노입자 개수농도분포 측정특성 비교)

  • Kim, M.S.;Kwon, J.W.;Chung, M.C.;Lee, J.W.
    • Journal of ILASS-Korea
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    • v.17 no.4
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    • pp.185-191
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    • 2012
  • Particulate matters (PM) that is generated by most diesel engine is regulated by the mass concentration measured by the conventional method it had been. Recently, Europe PMP (Particle Measurement Program) decided to start the regulation of vehicle's nano-sized particle number (PN) from the year of 2011 because of nano-particle's higher degree of harm to the human body. So firstly, the standard level of PN emission is introduced in the Euro 5/6 emissions regulation with a limit of $6{\times}10^{11}$ per km for light duty vehicle. Also KPMP(Korea Particle Measurement Program) was organized to copy quickly international technical trend. In this paper, it was investigated the nano-sized PN measurement characteristics for different particle generators between spray type and soot type. And the difference ratio between particle generators, the characteristic of PN concentration, counting efficiency and linearity was analyzed. Then, we make conclusions as followed. When particle diameter is increased, counting efficiency of two generators is decreased. Also Secondary calibration method is more higher 3% than Primary calibration method. Finally, SOF which is included in soot particles is not totally removed so it have great influence on test result of counting efficiency and linearity.

Simultaneous Kinetic Spectrophotometric Determination of Sulfite and Sulfide Using Partial Least Squares (PLS) Regression

  • Afkhami, Abbas;Sarlak, Nahid;Zarei, Ali Reza;Madrakian, Tayyebeh
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.863-868
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    • 2006
  • The partial least squares (PLS-1) calibration model based on spectrophotometric measurement, for the simultaneous determination of sulfite and sulfide is described. This method is based on the difference between the rate of the reaction of sulfide and sulfite with Malachite Green in pH 7.0 buffer solution and at 25 ${^{\circ}C}$. The absorption kinetic profiles of the solutions were monitored by measuring the decrease in the absorbance of Malachite Green at 617 nm in the time range 10-180 s after initiation of the reactions with 2 s intervals. The experimental calibration matrix for partial least squares (PLS-1) calibration was designed with 24 samples. The cross-validation method was used for selecting the number of factors. The results showed that simultaneous determination could be performed in the range 0.030-1.5 and 0.030-1.2 $\mu$g m$L ^{-1}$ for sulfite and sulfide, respectively. The proposed method was successfully applied to simultaneous determination of sulfite and sulfide in water samples and whole human blood.

Mathematical Modeling for Calculating the Vertical Air Temperature Distribution in an Atrium Space (아트리움 공간의 수직공기온도분포 계산을 위한 수학모형의 작성)

  • 박종수;안병욱
    • Korean Journal of Air-Conditioning and Refrigeration Engineering
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    • v.15 no.6
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    • pp.533-542
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    • 2003
  • This study aims to propose a simplified mathematical model for calculating vertical air temperature distribution in a four-sided atrium. In the first stage of the mathematical modeling, the computer model combined zonal model and solar radiation model using Monte Carlo method and Ray tracing technique went through a computer simulation with architectural variables applied to a four-sided atrium in summer. In the next stage, Curve Expert, a computer program that gets the most suitable solution ac-cording to the least squares method, is used to analyze the results of the computer simulation and to derive the mathematical model. The accuracy of the mathematical model was evaluated through a comparison of calculation results from a mathematical model and computer simulation. In this validation step using the least square method, the R2 value of the Zones 1, 2 and 3 showed higher than 0.945. Zone 4 has an R2 value of 0.911, lower than the previous three zones. However the relative error was below 0.5%, which is considered very small.

Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of ε-Acetamidocaproic Acid in Rat Plasma

  • Kim, Tae Hyun;Choi, Yong Seok;Choi, Young Hee;Kim, Yoon Gyoon
    • Toxicological Research
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    • v.29 no.3
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    • pp.203-209
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    • 2013
  • A simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of ${\varepsilon}$-acetamidocaproic acid (AACA), the primary metabolite of zinc acexamate (ZAC), in rat plasma by using normetanephrine as an internal standard. Sample preparation involved protein precipitation using methanol. Separation was achieved on a Gemini-NX $C_{18}$ column ($150mm{\times}2.0mm$, i.d., 3 ${\mu}m$ particle size) using a mixture of 0.1% formic acid-water : acetonitrile (80 : 20, v/v) as the mobile phase at a flow rate of 200 ${\mu}l/min$. Quantification was performed on a triple quadrupole mass spectrometer employing electrospray ionization and operating in multiple reaction monitoring (MRM) and positive ion mode. The total chromatographic run time was 4.0 min, and the calibration curves of AACA were linear over the concentration range of 20~5000 ng/ml in rat plasma. The coefficient of variation and relative error at four QC levels were ranged from 1.0% to 5.8% and from -8.4% to 6.6%, respectively. The present method was successfully applied for estimating the pharmacokinetic parameters of AACA following intravenous or oral administration of ZAC to rats.

Study on the Error Compensation in Strain Measurement of Sheet Metal Forming (박판성형 변형률 측정 오차보정에 관한 연구)

  • 한병엽;차지혜;금영탁
    • Proceedings of the Korean Society for Technology of Plasticity Conference
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    • 2003.05a
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    • pp.270-273
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    • 2003
  • The strain measurement of the panel in the sheet metal forming is essential work which provides experimental data needed to die design, process design, and product inspection. To measure efficiently the complex geometry strain, the 3-dimensional automative strain measurement system, which has high accuracy in theory, but has some 3∼5% errors in practice, is often used. The object of this study is to develop the error compensation technology to eliminate the strain, errors resulted when formed panels are measured using an automated strain measurement system. To achieve the study object, the position error calibration method correcting coordinates of the grid node recognized by a camera using error functions is suggested. Then the position errors were found by calculating the difference in the position of the cube node between real coordinates and measured coordinates in toms of node coordinates and the error calibration equations were derived by regressing the position errors. In order to show the validation of the suggested position error calibration method, finite element analysis and current calibration method was performed for the initial-blankformed.

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Determination of amitraz by high-performance Liquid chromatography with photodiode array detection and method validation (HPLC-PDA를 이용한 Amitraz의 분석법 확립 및 검증)

  • Yun, Hyeong-Jun;Yun, So-Mi;Lee, Myoung-Heon;Son, Seong-Wan
    • Korean Journal of Veterinary Research
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    • v.48 no.1
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    • pp.33-38
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    • 2008
  • In veterinary medicine amitraz has been used as an insecticide to eliminates mites, lice, and ticks in dogs, cats, goats, swine and cattle. The objective of present study was to developed an analytical method using one-step extraction and determination of the amitraz in veterinary drugs by liquid chromatography (LC). The amitraz was analyzed by LC equipped with Waters XTerra RP18 ($4.8{\times}250mm;\;5{\mu}m;\;Waters,\;USA$) analytical column, using 75% acetonitrile (acetonitrile/D.W; 75/25) at 1.0 ml/ min. The UV-VIS detection of amitraz was made at 290 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $80{\sim}120{\mu}g/ml$. The limit of detection was $0.09{\mu}g/ml $ and limit of quantification was $0.27{\mu}g/ml $. The method showed good intra-day precision (CV 0.05~0.09%) and inter-day precision (CV 0.06~0.18%).