• Title/Summary/Keyword: analytical validation

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Development and validation of an analytical method for the quantification of 2,6-diisopropylnaphthalene in agricultural products using GC-MS/MS

  • Lee, Han Sol;Park, Ji-Su;Lee, Su Jung;Shin, Hye-Sun;Chung, Yun mi;Choi, Ha na;Yun, Sang Soon;Jung, Yong-hyun;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.1-8
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    • 2021
  • An analytical method was developed and optimized for the quantification of a plant growth regulator, 2,6-diisopropylnaphthalene (2,6-DIPN), in agricultural products using gas chromatography-tandem mass spectrometry. The samples were extracted, partitioned, and were purified using a Florisil® cartridge. To validate the analytical method, its specificity, linearity, limit of detection (LOD) and limit of quantification (LOQ) of the instrument, LOQ of the analytical method (MLOQ), accuracy, and repeatability were considered. The method displayed excellent results during validation, and is suitable for the determination and quantification of the low residual levels of the analyte in the agricultural samples. All of the results with the optimized method were satisfactory and within the criteria ranges requested in the Codex Alimentarius Commission guidelines and the Ministry of Food and Drug Safety guidelines for pesticide residue analysis. The developed method is simple and accurate and can be used as a basis for safety management of 2,6-DIPN.

Quality Control System for Analytical Chemistry Laboratory of Pesticide Products (농약 이화학시험 분석기관 정도관리체계)

  • Chang, Hee-Ra;Lee, Joon-Yeob;Lee, Young-Ju;Kang, Hye-Rim;Kim, Chan-Sub;Kim, Kyun
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.529-544
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    • 2011
  • Many international organizations, such as the International Organization for Standardization (ISO) and Collaborative International Pesticide Analytical Council (CIPAC), have published a guide to quality control requirements, proficiency testing and method validation for pesticide formulation. In general, proficiency testing is to determine the performance of individual laboratories from the comparison of test results and to monitor a laboratory's performance abilities. One of quality assurance (QA) scheme would be include the validation of analytical method that implies a performance characteristics, specificity, selectivity, linearity and so on. According to many international organizations, the quantification methods of active substance in formulated pesticide products are required to be reproducible, accurate and precise. This study was conducted to compare the international guidelines for the quality control, proficiency testing and method validation of analytical laboratories and to propose a general guidance for the establishment of quality control system in the analytical chemistry laboratories of pesticide formulation in domestic.

Development and validation of a HPLC method for the simultaneous determination of chlorquinaldol and promestriene in complex prescription (복방제제 내 클로르퀴날돌과 프로메스트리엔에 대한 HPLC 기반 동시분석법의 개발 및 밸리데이션)

  • Lee, Seul-Ji;Shin, Sang-Yeon;Shin, Hae-Jin;Lee, Jin-Gyun;Kim, Dong-Hwan;Lee, Su-Jung;Han, Sang-Beom;Park, Jeong-Hill;Lee, Jeong-Mi;Kwon, Sung-Won
    • Analytical Science and Technology
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    • v.25 no.2
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    • pp.152-157
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    • 2012
  • Currently, many types of compound preparations are being used but the quality control guidelines for their use are lacking. In case of single compound drug, the quality control methods are specified in the pharmacopeia. However, there is no method to simultaneously analyze compound preparations. In this study, a simple validated analytical method for HPLC separation of chlorquinaldol and promestriene is introduced. Validation was divided into categories including linearity, precision, accuracy (recovery) and system suitability. The contents of the products which are on the market were monitored using the validated analytical method and the robustness of the analytical method was tested by conducting an inter-laboratory validation.

Analytical method validation of oxiracetam using HPLC (HPLC를 이용한 의약품 주성분인 옥시라세탐의 Analytical Method Validation)

  • Kim, Yoo-Gon;Seo, Houng-Seok;Won, Chan-Hee
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.587-594
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    • 2010
  • This study aims to determine that the test of medicines containing oxiracetam as their main ingredient was properly performed according to protocol. Furthermore, the study is to provide the written form of protocol in order to examine the validity of the HPLC analytical method for the quantitative analysis of oxiracetam in the finished products. In this experiment, system suitability, precision, linearity, range, accuracy, specificity, quantitative limit, and detection limit of the analytical method which was used to determine the contained quality of oxiracetam, were examined. The result shows that system suitability indicates 0.127% RSD, plate number 15081, tailing factor 0.49, and resolution 32.41. The experiment of precision reveals the result of below 0.359% for repetitiveness and among the subjects. In the linearity experiment, a coefficient of correlation ($R^2$) indicates that it is 1. The accuracy experiment satisfies the standards of the recovery test, which is minimum 98.4% and maximum 99.6%. Detection limit is 0.1 mg/L and quantitative limit was found to be 0.5 mg/L. The experiment to check the specificity also satisfies the standards, so the finished product using oxiracetam as the main ingredient is verified as suitable.

Comparison of Performance of Models to Predict Hardness of Tomato using Spectroscopic Data of Reflectance and Transmittance (토마토 반사광과 투과광 스펙트럼 분석에 의한 경도 예측 성능 비교)

  • Kim, Young-Tae;Suh, Sang-Ryong
    • Journal of Biosystems Engineering
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    • v.33 no.1
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    • pp.63-68
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    • 2008
  • This study was carried out to find a useful method to predict hardness of tomato using optical spectrum data. Optical spectrum of reflectance and transmittance data were collected processed by 9 kind of preprocessing methods-normalizations of mean, maximum and range, SNV (standard normal variate), MSC (multiplicative scatter correction), the first derivative and second derivative of Savitzky-Golay and Norris-Gap. With the preprocessed and non-processed original spectrum data, prediction models of hardness of tomato were developed using analytical tools of PLS (partial least squares) and MLR (multiple linear regression) and tested for their validation. The test of validation resulted that the analytical tools of PLS and MLR output similar performances while the transmittance spectra showed much better result than the reflectance spectra.

A Simulation Study on Regularization Method for Generating Non-Destructive Depth Profiles from Angle-Resolved XPS Data

  • Ro, Chul-Un
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.707-714
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    • 1995
  • Two types of regularization method (singular system and HMP approaches) for generating depth-concentration profiles from angle-resolved XPS data were evaluated. Both approaches showed qualitatively similar results although they employed different numerical algorithms. The application of the regularization method to simulated data demonstrates its excellent utility for the complex depth profile system. It includes the stable restoration of the depth-concentration profiles from the data with considerable random error and the self choice of smoothing parameter that is imperative for the successful application of the regularization method. The self choice of smoothing parameter is based on generalized cross-validation method which lets the data themselves choose the optimal value of the parameter.

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Simultaneous Determination of Four Compounds from Cercidiphyllum japonicum Using HPLC-UV Analysis

  • Kang, Jeongyeon;Jang, Hyeon Seok;Kim, Ju Yeol;Lee, Min Sung;Bae, Young Soo;Kwon, Yongsoo;Yang, Heejung
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.280-283
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    • 2021
  • Cercidiphyllum japonicum is being used for the treatment of obesity and liver fibrosis in Korean local clinics. In the present study, we tried to develop an analytical methodology for the determination of the chemical markers of Cercidiphyllum japonicum. Four chemicals, maltol (1), chlorogenic acid (2), quercetin (3), and avicularin (4), were selected for method validation, and the analytical conditions were optimized and validated using high-performance liquid chromatography coupled with an ultraviolet detector (HPLC-UV). Additionally, the seasonal variations of four markers were monitored every month for six months. The contents of four chemicals markers were most detected in a sample collected in June.

HFFB technique and its validation studies

  • Xie, Jiming;Garber, Jason
    • Wind and Structures
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    • v.18 no.4
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    • pp.375-389
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    • 2014
  • The high-frequency force-balance (HFFB) technique and its subsequent improvements are reviewed in this paper, including a discussion about nonlinear mode shape corrections, multi-force balance measurements, and using HFFB model to identify aeroelastic parameters. To apply the HFFB technique in engineering practice, various validation studies have been conducted. This paper presents the results from an analytical validation study for a simple building with nonlinear mode shapes, three experimental validation studies for more complicated buildings, and a field measurement comparison for a super-tall building in Hong Kong. The results of these validations confirm that the improved HFFB technique is generally adequate for engineering applications. Some technical limitations of HFFB are also discussed in this paper, especially for higher-order mode response that could be considerable for super tall buildings.

Wound-State Monitoring for Burn Patients Using E-Nose/SPME System

  • Byun, Hyung-Gi;Persaud, Krishna C.;Pisanelli, Anna Maria
    • ETRI Journal
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    • v.32 no.3
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    • pp.440-446
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    • 2010
  • Array-based gas sensors now offer the potential of a robust analytical approach to odor measurement for medical use. We are developing a fast reliable method for detection of microbial infection by monitoring the headspace from the infected wound. In this paper, we present initial results obtained from wound-state monitoring for burn patients using an electronic nose incorporating an automated solid-phase microextraction (SPME) desorption system to enable the system to be used for clinical validation. SPME preconcentration is used for sampling of the headspace air and the response of the sensor module to variable concentrations of volatiles emitted from SPME fiber is evaluated. Gas chromatography-mass spectrometry studies prove that living bacteria, the typical infectious agents in clinical practice, can be distinguished from each other by means of a limited set of key volatile products. Principal component analysis results give the first indication that infected patients may be distinguished from uninfected patients. Microbial laboratory analysis using clinical samples verifies the performance of the system.

Development of Asbestos Quality Control Sample for Proficiency Analytical Testing 1 - Development of Manufacturing Apparatus and Sample Preparing Procedure for Asbestos Quality Control Sample - (석면분석 정도관리용 표준시료 개발연구 I - 석면분석 정도관리용 표준시료 제조장치 개발 및 시료제조 방법 확립 -)

  • Yi, Gwang Yong;Lee, Jong- Han;Jung, Sijeong;Park, Doo Yong
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.19 no.2
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    • pp.81-87
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    • 2009
  • Final purpose of this study was designed to develop the quality control(QC) sample for proficiency analytical testing of asbestos. This study consisted of two parts; first, development of manufacturing apparatus and sample preparing procedure for asbestos quality control(QC) sample: second, validation of the QC samples made by our developed method as asbestos proficiency analytical testing sample. The main results of the first part research are as followed We developed the apparatus for manufacturing the asbestos QC sample, consisted of filter hold, filter holder manifolder, vacuum system, and vacuum pump. The most proper filter of making the QC samples was a cellulose ester membrane filter with 25 mm diameter, pore size 0.8 um. And we presented the optimal procedure for preparing the asbestos QC sample by using the developed apparatus. We will verify the manufactured asbestos QC samples by this method, and present the validation results to confirm the reliability as a asbestos QC sample in next paper.