• Title/Summary/Keyword: method validation #5

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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%).

Multiresidue Determination of Quinolones in Porcine, Chicken, and Bovine Muscle Using Liquid Chromatography with Fluorescence Detection

  • Lee, Sang-Hee;Shim, You-Sin;Kim, Hyun-Ju;Shin, Dong-Bin
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.978-984
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    • 2009
  • An analytical method for the simultaneous determination of 9 quinolones (QNs) in porcine, chicken, and bovine muscles was developed and validated using liquid chromatography-fluorescence detector (LC-FLD). The samples were extracted using a liquid-liquid extraction (LLE) process. Chromatographic separation was achieved on a reverse phase $C_8$ column with a gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and acetonitrile (ACN). The proposed method was validated according to the Food and Drug Administration (FDA) guideline for bioanalytical assay procedures. Recoveries of QNs were 83.1-111.9% with relative standard deviations (RSDs) below 15%. Linearity within a range of 30-500 ${\mu}g/kg$ was obtained with the correlation coefficient ($R^2$) of 0.9967-0.9999. The limits of detection (LOD) were 1-16 ${\mu}g/kg$. These values were lower than the maximum residues limits (MRLs) established by the European Union (EU). The present method was successfully applied to determine QNs in edible muscles.

Estimation of Formability for Sheet Metal Forming of Electronic Parts (전자 박판 부품의 가공성 평가에 대한 연구)

  • Lee, B.C.;Kang, S.Y.;Moon, J.H.
    • Journal of the Korean Society for Precision Engineering
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    • v.13 no.5
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    • pp.104-114
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    • 1996
  • For the improvement of productivity, the reduction of cost and time for manufacturing is mandatory, especially in the field of electromic industry. The study is concerned with a practical means of systematic assistance to formability estimation and selection of reliable design specification for electronic sheet metal parts. The objective of this research work is to develop a simulation system which hops to analyze the target processes with the finite element method and to acquire available design data quickly and exactly. The simulation system developed in the study consists of design verification, selection of optimal combination of parameters, knowledge acquisition and graphical user interface(GUI). Design verification is automatically carried out by using the finite element method. A data base management system and nomograms are utilized for knowledge acquisition. The developed system has been applied to some major sheet metal forming operations such as flanging, embossing, bending and blanking. According to the simulated results, the validation of the target processes has been confirmend. Analysis data, estimation rules of formability and graphical representation of the analysis have been employed for the designer's understanding and evaluation, thus providing a practical means of robust design and evaluation of forma- bility for producing electronic sheet metal parts.

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Effect of particle size and scanning cup type for near infrared reflection on the soil property measurement

  • Ryu, Kwan-Shig;Cho, Rae-Kwang;Park, Woo-Churl;Kim, Bok-Jin
    • Near Infrared Analysis
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    • v.1 no.2
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    • pp.35-39
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    • 2000
  • The purpose of this research was to find out suitable soil sample preparation and sample holding tools for NIR reflection radiation for estimating soil components. NIR reflectance was scanned at 2nm intervals from 1,100 to 2,500nm with an InfraAlyzer 500(Bran+Luebbe Co.). Coarse(2.0mm) and fine(0.5mm) soil sample and various sample holding tools were used to obtain mean diffuse reflection of the soil for the calibration and validation of the calibration set in estimating moisture, organic matter and total nitrogen of the soils. Multiple linear regression was used to obtain the best correlation of NIR spectroscopy method. Correlation of NIR spectroscopy method. Correlation of NIR spectra for finely and coarsely sized soil did not show much difference. The standard errors of prediction(SE) using different types of sample holding tools for organic matter, total nitrogen and soil moisture were better than 0.765, 0.041 and 0.63% respectively. From the results it can be concluded that NIR spectroscopy with flow type cell could be used as a fast routine testing method in quantitative determination of organic matter, total nitrogen and soil moisture.

Liquid Chromatography-Tandem Mass Spectrometry Analysis of Riboflavin in Beagle Dog Plasma for Pharmacokinetic Studies

  • Jeong, Hyeon Myeong;Shin, Beom Soo;Shin, Soyoung
    • Mass Spectrometry Letters
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    • v.11 no.1
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    • pp.10-14
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    • 2020
  • Riboflavin is a water-soluble vitamin, which serves as a precursor to flavin mononucleotide and flavin adenine dinucleotide. This study aimed to develop a simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis for the quantification of riboflavin in the Beagle dog plasma. This method utilized simple protein precipitation with acetonitrile and 13C4, 15N2-riboflavin was used as an internal standard (IS). For chromatographic separation, a hydrophilic interaction liquid chromatography (HILIC) column was used with gradient elution. The mobile phase consisted of 0.1% (v/v) aqueous formic acid with 10 mM ammonium formate and acetonitrile with 0.1% (v/v) formic acid. Since riboflavin is an endogenous compound, 4% bovine serum albumin in phosphate buffered saline was used as a surrogate matrix to prepare the calibration curve. The quantification limit for riboflavin in the Beagle dog plasma was 5 ng/mL. The method was fully validated for its specificity, sensitivity, accuracy and precision, recovery, and stability according to the US FDA guidance. The developed LC-MS/MS method may be useful for the in vivo pharmacokinetic studies of riboflavin.

Development and validation of a selective and sensitive LC-MS/MS method for determination of misoprostol acid in human plasma: Application to bioequivalence study

  • Park, Yong Sun;Kim, Keun Nam;Kim, Ye Na;Kim, Jung Hwan;Kim, Jin Young;Sim, Soo Ji;Lee, Heon Soo
    • Analytical Science and Technology
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    • v.28 no.1
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    • pp.17-25
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    • 2015
  • A rapid, sensitive and specific method was developed and validated using electrospray ionization (ESI) tandem mass spectrometry (LC-MS/MS) for determination of misoprostol acid in human plasma. Misoprostol $acid-d_5$ was used as in internal standard (IS). The analyte and IS were extracted by simple one step solid phase extraction (SPE). Linearity in plasma was obtained over the concentration range 10~3000 pg/mL and lower limit of quantification (LLOQ) was identifiable and reproducible at 10 pg/mL. The intra- and inter-day precision values were below 9% and the accuracy was ranged from 93.81% to 102.02% at all four quality control samples. The method was has been successfully applied for routine assay to support pharmacokinetic study of misoprostol acid in human plasma after an oral administration of 0.4 mg misoprostol.

DEVELOPMENT OF A CORE THERMO-FLUID ANALYSIS CODE FOR PRISMATIC GAS COOLED REACTORS

  • Tak, Nam-Il;Lee, Sung Nam;Kim, Min-Hwan;Lim, Hong Sik;Noh, Jae Man
    • Nuclear Engineering and Technology
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    • v.46 no.5
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    • pp.641-654
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    • 2014
  • A new computer code, named CORONA (Core Reliable Optimization and thermo-fluid Network Analysis), was developed for the core thermo-fluid analysis of a prismatic gas cooled reactor. The CORONA code is targeted for whole-core thermo-fluid analysis of a prismatic gas cooled reactor, with fast computation and reasonable accuracy. In order to achieve this target, the development of CORONA focused on (1) an efficient numerical method, (2) efficient grid generation, and (3) parallel computation. The key idea for the efficient numerical method of CORONA is to solve a three-dimensional solid heat conduction equation combined with one-dimensional fluid flow network equations. The typical difficulties in generating computational grids for a whole core analysis were overcome by using a basic unit cell concept. A fast calculation was finally achieved by a block-wise parallel computation method. The objective of the present paper is to summarize the motivation and strategy, numerical approaches, verification and validation, parallel computation, and perspective of the CORONA code.

Validation of Extended Building Heat Transfer Model (건축전열모델의 확장에 관한 연구)

  • 조민관
    • Korean Journal of Air-Conditioning and Refrigeration Engineering
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    • v.15 no.5
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    • pp.422-431
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    • 2003
  • Theory of the building heat transfer is generally limited to the heat flux to the surfaces of windows and walls, which influences the indoor climate of a building, in the field of architectural environmental engineering. While the heat flux from the buildings to their environment has been considered in the viewpoint of urban climate, its conventional theory have been rarely examined. The purpose of this study is to propose a building-urban heat transfer model for defining the relation between the building and the urban climate by extending the building heat transfer model. In this study, the extended building heat transfer model, where response factor method is used, is established on the urban space and the indoor space by the boundary of building envelopes. Computer simulation (HASP/ACLD) is conducted on the subjected urban area by the established building-urban heat transfer model. As a result it is logically proved that the short waves of solar radiation, which interact with long Waves of radiation from the buildings and the earth, increase the urban air temperature ana buildings largely influence on the urban climate.

Quantitative Determination of Amitriptyline and Its Metabolite in Rat Plasma by Liquid Chromatography-tandem Mass Spectrometry

  • Chae, Jung-Woo;Baek, In-Hwan;An, Jung-Hwa;Kim, Eun-Jung;Kwon, Kwang-Il
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2163-2167
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    • 2012
  • A rapid, specific, and reliable LC-MS/MS-based bioanalytical method was developed and validated in rat plasma for the simultaneous quantitation of amitriptyline and its metabolite nortriptyline. Chromatographic separation of these analytes was achieved on a Gemini C18 column ($50{\times}4.60mm$, $5{\mu}m$) using reversed-phase chromatography. The mobile phase was an isocratic solvent system consisting of 1% formic acid in water and methanol (10:90, v/v), at a flow rate of 0.2 mL/min. The analytical range was set as 0.1-500 ng/mL for amitriptyline and 0.08-500 ng/mL for nortriptyline using a $200{\mu}L$ plasma sample. The accuracy and precision of the assay were in accordance with FDA regulations for the validation of bioanalytical methods. The validated method was successfully applied to a pharmacokinetic study in six rats after oral administration of amitriptyline (15 mg/kg). This method allows laboratory scientists to rapidly determine amitriptyline and nortriptyline concentrations in plasma.

LC-MS/MS Assay Validation for a New Immune Modulator, JHL45, and its Major Metabolite in Plasma: Application to Pharmacokinetic Studies in Rats

  • Baek, In-Hwan;Chae, Jung-Woo;Song, Gyu-Yong;Kwon, Kwang-Il
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2631-2636
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    • 2009
  • JHL45, a novel immune modulator for anti-atopic dermatitis and allergic airway disease, was synthesized from decursin isolated from Angelica gigas. In order to conduct a pharmacokinetic study of JHL45, an analytical method, ideally one that uses a minimal amount of biological sample must first be validated. In this study, a HPLC-MS/MS method was developed and validated for the quantification of JHL45 and its major metabolite, (+)-decursinol, from 10 ${\mu}L$ of rat plasma. JHL45 was stable under the analysis conditions, and intra- and inter-day accuracies exceeded 90.06%, with a precision variability ${\leq}$ 13.16% for each analyte. The mean values for Cmax, AUC8h, half-life of JHL45 in rats after intravenous administration of 5 mg/kg JHL45 were 24.59 μg/mL, 10.02 ${\mu}g{\cdot}h/mL$, and 1.88 h, respectively. The validated method herein will be useful for further pharmacokinetic studies of JHL45, as well as in preclinical and clinical phases.