• Title/Summary/Keyword: Analytical validation

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Parametric Studies on the Sensitivity of Single Isolated Aluminum Particle Combustion Modeling (알루미늄 입자 연소 지배인자의 민감도 해석)

  • Lee, Sang-Hyup;Ko, Tae-Ho;Yang, Hee-Sung;Yoon, Woong-Sup
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2010.11a
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    • pp.321-327
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    • 2010
  • A simplified analytical modeling for micro-sized single metal particle combustion in air was conducted in the present study. The metal particle combustion consists of two distinct reaction regimes, ignition and quasi-steady burning, and the thermo-fluidic phenomena in each stage are formulated by virtue of the conservation and transport equations. Reliability of the model is shown by rigorous validation of the method with emphasis laid on the characterizing the commanding parameters. Effects of Initial particle size, initial oxide film thickness, convection, ambient pressure and temperature are examined and addressed with validation.

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Validation and measurement uncertainty of HPLC-UV method for quercetin quantification in various foods

  • Seo, Eunbin;Lim, Suji;Yun, Choong-In;Shin, Jae-Wook;Kim, Young-Jun
    • Korean Journal of Food Science and Technology
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    • v.53 no.6
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    • pp.682-687
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    • 2021
  • The purpose of this study was to validate a high-performance liquid chromatography (HPLC) method for the quantitative analysis of quercetin in various foods. The method was based on HPLC-UV (360 nm). The method was validated using candy, beverage, and sausage which were tested for specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy, and the measurement uncertainty was assessed. Matrix-matched calibration was also applied. The calibration curves (0.5-50 mg/L) showed good linearity (r2≥0.9998). LOD and LOQ ranged from 0.15 to 0.31 mg/kg and from 0.44 to 0.93 mg/kg, respectively. The average accuracy and precision at 0.5, 2.5, and 10 mg/kg ranged from 84.3 to 102.0% and 0.7 to 3.0 relative standard deviation (RSD%), respectively. This study confirmed the applicability of the proposed method by applying it to commercial products, such as teas and beverages. Thus, the proposed analytical method is suitable for quantifying quercetin in various foods.

Validation of an HPLC/UV-based method for Salicornia herbacea-derived isorhamnetin-3-O-glucoside and quercetin-3-O-glucoside quantification

  • Park, Jun Yeon;Paje, Leo Adrianne;Kang, Ki Sung;Lee, Sanghyun
    • Journal of Applied Biological Chemistry
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    • v.64 no.3
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    • pp.285-290
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    • 2021
  • Salicornia herbacea is a type of salt marsh plant that has been used in traditional medicine to treat several diseases. Isorhamnetin-3-O-glucoside (I3G) and quercetin-3-O-glucoside (Q3G) are major flavonoids in S. herbacea that are known to exert various pharmacological activities. Therefore, our study sought to validate and optimize an HPLC/UV-based analytical method for I3G and Q3G yield quantification, as well as to determine its limit of detection, limit of quantification, linearity, precision, and accuracy. Upon testing a concentration range of 31.5-1.9 ㎍/mL the results exhibited good linearity (r2 ≥0.9996 and r2 ≥0.9999 for I3G and Q3G, respectively), and the procedure was deemed precise (relative standard deviation of ≤3.19 and ≤3.85%, respectively), and accurate (102.6-105.0 and 92.9-95.2%, respectively). The results showed that our proposed method could be used for rapid I3G and Q3G evaluation in S. herbacea.

Development and Validation of Quantitative Analysis Method for Phenanthrenes in Peels of the Dioscorea Genus

  • Kim, Hunseong;Cao, Thao Quyen;Yeo, Chae-eun;Shin, Seung Ho;Kim, Hiyoung;Hong, Dong-Hyuck;Hahn, Dongyup
    • Journal of Microbiology and Biotechnology
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    • v.32 no.8
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    • pp.976-981
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    • 2022
  • Phenanthrenes are bioactive phenolic compounds found in genus Dioscorea, in which they are distributed more in peel than in flesh. Recent studies on phenanthrenes from Dioscorea sp. peels have revealed the potential for valuable biomaterials. Herein, an analytical method using high-performance liquid chromatography (HPLC) for quantitation of bioactive phenanthrenes was developed and validated. The calibration curves were obtained using the phenanthrenes (1-3) previously isolated from Dioscorea batatas concentrations in the range of 0.625-20.00 ㎍/ml with a satisfactory coefficient of determination (R2) of 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) values of the isolated phenanthrenes ranged from 0.78-0.89 and 2.38-2.71 ㎍/ml, respectively. The intraday and interday precision ranged from 0.25-7.58%. The recoveries of the isolated phenanthrenes were from 95 to 100% at concentrations of 1.25, 2.5, and 5.0 ㎍/ml. Additionally, phenanthrenes (1-3) were found in all investigated peel extracts. Hence, the developed method was encouraging for the quantitative analysis of phenanthrenes in genus Dioscorea.

Simulation, design optimization, and experimental validation of a silver SPND for neutron flux mapping in the Tehran MTR

  • Saghafi, Mahdi;Ayyoubzadeh, Seyed Mohsen;Terman, Mohammad Sadegh
    • Nuclear Engineering and Technology
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    • v.52 no.12
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    • pp.2852-2859
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    • 2020
  • This paper deals with the simulation-based design optimization and experimental validation of the characteristics of an in-core silver Self-Powered Neutron Detector (SPND). Optimized dimensions of the SPND are determined by combining Monte Carlo simulations and analytical methods. As a first step, the Monte Carlo transport code MCNPX is used to follow the trajectory and fate of the neutrons emitted from an external source. This simulation is able to seamlessly integrate various phenomena, including neutron slowing-down and shielding effects. Then, the expected number of beta particles and their energy spectrum following a neutron capture reaction in the silver emitter are fetched from the TENDEL database using the JANIS software interface and integrated with the data from the first step to yield the origin and spectrum of the source electrons. Eventually, the MCNPX transport code is used for the Monte Carlo calculation of the ballistic current of beta particles in the various regions of the SPND. Then, the output current and the maximum insulator thickness to avoid breakdown are determined. The optimum design of the SPND is then manufactured and experimental tests are conducted. The calculated design parameters of this detector have been found in good agreement with the obtained experimental results.

Development of Simultaneous Analytical Method for Five Lignans in Edible Seeds (종자류 식품에 함유된 5종 리그난의 동시 분석법 개발)

  • Yoonjeong, Kim;Jiye, Pyeon;In-hwan, Baek;Younghwa, Kim
    • The Korean Journal of Food And Nutrition
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    • v.35 no.6
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    • pp.543-551
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    • 2022
  • There has been increased interest in lignans due to their potential effect in reducing the risk of developing several diseases. To evaluate lignan contents, sensitive and accurate methods should be developed for their quantification in food. The present study aimed to validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantification of 5 lignans: lariciresinol (Lar), matairesinol (Mat), pinoresinol (Pin), secoisolariciresinol (Seco), and syringaresinol (Syr). The validation included selectivity, linearity, recovery, accuracy, and precision. The method was proved to be specific, with a linear response (R2≥0.99). The limits of detection were 0.040~0.765 ㎍/100 g and the limits of quantification were 0.114~1.532 ㎍/100 g. Recoveries were 90.588~109.053% for black sesame powder. Relative standard deviations of repeatability and reproducibility were below 5%. Total lignan contents of roasted coffee bean, oat, and blacksoy bean were 105.702 ㎍/100 g, 78.965 ㎍/100 g, and 165.521 ㎍/100 g, respectively. These results showed that LC-MS/MS analysis would be effective in producing acceptable sensitivity, accuracy, and precision in five lignan analyses.

Comparison of Extraction Methods for Determination of Vitamin K1 in Vegetables (채소류의 비타민 K1 분석을 위한 추출방법의 비교)

  • Kim, Hyeongi;Choi, Youngmin;Cho, Young-Sook;Sung, Jeehye;Ham, Hyeonmi;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.11
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    • pp.1791-1795
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    • 2014
  • The objective of this study was to compare two extraction methods for determination of vitamin K1 (phylloquinone) in vegetables. In addition, analytical method validation parameters such as accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity were calculated to ensure the method's validity. Vitamin K1 was quantified by reversed-phase HPLC using post-column derivatization and fluorescence detection ($Ex{\lambda}=243nm$, $Ex{\lambda}=430nm$). Higher analytical values were observed using solvent extraction compared to those from the enzyme extraction method. The results from the method validation showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ were 0.1335 and 0.2784 ng/injection volume ($50{\mu}L$), respectively. The inter-day precision and inter-day precision were 2.0% and 2.1%, respectively. Overall recovery was close to 100% (n=5). The phylloquinone contents ranged from 9.42 to $1,212.57{\mu}g/100g$. Our study provides reliable data on the phylloquinone contents in commonly consumed vegetables in Korea.

Prediction and analysis of acute fish toxicity of pesticides to the rainbow trout using 2D-QSAR (2D-QSAR방법을 이용한 농약류의 무지개 송어 급성 어독성 분석 및 예측)

  • Song, In-Sik;Cha, Ji-Young;Lee, Sung-Kwang
    • Analytical Science and Technology
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    • v.24 no.6
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    • pp.544-555
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    • 2011
  • The acute toxicity in the rainbow trout (Oncorhynchus mykiss) was analyzed and predicted using quantitative structure-activity relationships (QSAR). The aquatic toxicity, 96h $LC_{50}$ (median lethal concentration) of 275 organic pesticides, was obtained from EU-funded project DEMETRA. Prediction models were derived from 558 2D molecular descriptors, calculated in PreADMET. The linear (multiple linear regression) and nonlinear (support vector machine and artificial neural network) learning methods were optimized by taking into account the statistical parameters between the experimental and predicted p$LC_{50}$. After preprocessing, population based forward selection were used to select the best subsets of descriptors in the learning methods including 5-fold cross-validation procedure. The support vector machine model was used as the best model ($R^2_{CV}$=0.677, RMSECV=0.887, MSECV=0.674) and also correctly classified 87% for the training set according to EU regulation criteria. The MLR model could describe the structural characteristics of toxic chemicals and interaction with lipid membrane of fish. All the developed models were validated by 5 fold cross-validation and Y-scrambling test.

Validation on the Analytical Method of Ginsenosides in Red Ginseng

  • Cho B. G.;Nho K. B.;Shon H. J.;Choi K. J.;Lee S. K.;Kim S. C;Ko S. R.;Xie P. S.;Yan Y. Z.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.491-501
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    • 2002
  • A cross-examination between KT&G Central Research Institute and Guangzhou Institute for Drug Control was carried out in order to select optimum conditions for extraction, separation and determination of ginsenosides in red ginseng and to propose a better method for the quantitative analysis of ginsenosides. The optimum extraction conditions of ginsenosides from red ginseng were as follows: the extraction solvent, $70\%$ methanol; the extraction temperature, $100^{\circ}C;$ the extraction time, 1 hour for once; and the repetition of extraction, twice. The optimum separation conditions of ginsenosides on the SepPak $C_{18}$ cartridge were as follows: the loaded amount, 0.4 g of methanol extract; the washing solvents, distilled water of 25 ml at first and then $30\%$ methanol of 25 ml; the elution solvent, $90\%$ methanol of 5 ml. The optimum HPLC conditions for the determination of ginsenosides were as follows: column, Lichrosorb $NH_2(25{\times}0.4cm,$ 5${\mu}m$, Merck Co.); mobile phase, a mixture of acetonitrile/water/isopropanol (80/5/15) and acetonitrile/water/isopropanol (80/20/15) with gradient system; and the detector, ELSD. On the basis of the optimum conditions a method for the quantitative analysis of ginsenosides were proposed and another cross-examination was carried out for the validation of the selected analytical method conditions. The coefficient of variances (CVs) on the contents of ginsenoside-$Rg_{1}$, -Re and $-Rb_1$ were lower than $3\%$ and the recovery rates of ginsenosides were $89.4\~95.7\%,$ which suggests that the above extraction and separation conditions may be reproducible and reasonable. For the selected HPLC/ELSD conditions, the CVs on the detector responses of ginsenoside-Rg, -Re and $-Rb_1$) were also lower than $3\%$, the regression coefficients for the calibration curves of ginsenosides were higher than 0.99 and two adjacent ginsenoside peaks were well separated, which suggests that the above HPLC/ELSD conditions may be good enough for the determination of ginsenosides.

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Quantification of Tocopherol and Tocotrienol Content in Rice Bran by Near Infrated Reflectance Spectroscopy (근적외선분광분석기를 이용한 미강의 Tocopherol과 Tocotrienol 함량 분석)

  • 김용호;강창성;이영상
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.49 no.3
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    • pp.211-215
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    • 2004
  • Near infrared reflectance spectroscopy (NIRS) is a rapid and accurate analytical method for determining the composition of agricultural products and feeds. This study was conducted to determine tocopherol and tocotrienol contents in rice bran by using NIRS system. Total 80 rice bran samples previously analyzed by HPLC were scanned by NIRS and over 60 samples were selected for calibration and validation equation. A calibration equation calculated by MPLS(modified partial least squares) regression technique was developed and coefficient of determination for tocopheyol and tocotyienol content were 0.975 and 0.984, respectively, in calibration sets. Each calibration equation was fitted to validation set that was performed with the remaining samples not included is the calibration set, which showed high positive correlation both in tocopherol and tocotrienol content file. This results demonstrate that the developed NIRS equation can be practically used as a rapid screening method for quantification of tocopherol and tocotrienol contents in rice bran.