• 분석과학
• /
• 제34권1호
• /
• pp.1-8
• /
• 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.

• 농약과학회지
• /
• 제15권4호
• /
• pp.529-544
• /
• 2011

분석표준화 관련 국제기관인 ISO, CIPAC 등은 농약제품 시험기관에 대한 정도관리(QC), 숙련도 시험 및 분석법 검증을 수행하기 위한 요구조건을 지침서로 제시하고 있다. 일반적으로, 숙련도 시험은 시험기관의 분석능력 평가를 위하여 시험기관간 비교시험을 바탕으로 시험기관의 수행능력과 기술능력 정도를 판단할 수 있다. 분석법 검증 절차는 정도관리(QC)에서 중요한 단계 중 하나로 특이성, 선택성, 직선성 등의 항목들이 포함되며, 대부분의 국제기관이 농약제품 중 주요성분에 대한 정량분석법에서 재현성, 정확성 및 정밀성 등을 요구하고 있다. 본 연구에서는 농약 이화학시험 분석기관의 시험연구과정 및 결과에 대한 신뢰성을 높이기 위해 국내 외 정도관리에 관한 지침서를 비교 검토하여 국제적으로 표준화된 지침서에 적합한 구체적이고, 효율적인 농약 이화학시험 분석기관의 농약분석법 검증절차 및 시험기관 정도관리 체계(안)를 제안하고자 한다.

• 분석과학
• /
• 제25권2호
• /
• pp.152-157
• /
• 2012

현재 시중에 많은 복방제제가 유통되고 있음에도 불구하고 이의 품질관리를 위한 시험법은 부족한 실정이다. 여러 주효 성분을 가지는 복방제제의 경우 대부분 약전에 수재된 항목 중 2개 이상의 조합으로 구성되어 있으나 약전에 단일 항목에 대한 시험법이 고시되어 있을 뿐 여러 항목을 한번에 시험하는 방법이 없어 한가지 제제를 관리 하는 데에 여러 시험법이 요구되어 효율이 낮고 비용이 높다. 따라서 본 연구는 현재 유통중인 복방제제의 새로운 분석법을 개발한 과정과 그 때에 적용되는 기준을 제시하고 그 결과를 검증하였다. 복방 프로메스트리엔, 클로르퀴날돌 제제에 대한 새로운 분석법을 HPLC를 기반으로 가장 적용이 용이하게 개발하였으며 직선성, 정밀성, 정확성(회수율), 시스템 적합성(반복성, 분리도) 등의 항목에 대하여 밸리데이션을 수행함으로써 분석법을 검증하였다. 또한 개발된 시험법을 이용하여 시중 제품을 모니터링하고 실험실간 밸리데이션을 수행하여 시험법의 견고성을 확인함으로써 새로운 고시안으로서의 가능성을 제시하였다.

• 분석과학
• /
• 제23권6호
• /
• pp.587-594
• /
• 2010

완제품의 주성분인 옥시라세탐이 함유된 의약품의 시험법실시 계획서에 따른 시험이 적절히 진행되었는지 시험법의 검증여부를 하고 본 protocol이 완제품 중 옥시라세탐의 정량분석을 위한 HPLC 분석법의 타당성을 검증하기 위한 문서화된 절차를 제공하는 것을 목적으로 한다. 본 실험에서는 옥시라세탐 함량시험에 사용된 분석법에 대하여 시스템 적합성, 정밀성, 직선성, 범위, 정확도, 특이성, 정량한계, 검출한계에 대하여 확인하였다. 실험결과 시스템적합성에서 정밀도(RSD%) 0.127%이하, 이론단수 15081, tailing factor 0.49, 그리고 분리능 32.41을 나타내었고, 정밀도실험에서는 RSD% 0.359% 이하의 결과를 보였다. 그리고 직선성 실험에서는 상관계수($R^2$)가 1을 나타내었고, 정확도 실험에서는 recovery test로서 최소 98.4%, 최대 99.6%로 기준을 만족하였다. 검출한계는 0.1 mg/L이였으며, 정량한계는 0.5 mg/L이었다. 그리고 특이성 실험에 있어서도 기준을 만족하는 결과를 나타내어 옥시라세탐을 주성분으로 하는 완제의약품 시험법은 적합한 시험법임이 검증되었다.

• Journal of Biosystems Engineering
• /
• 제33권1호
• /
• pp.63-68
• /
• 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.

• 분석과학
• /
• 제8권4호
• /
• pp.707-714
• /
• 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.

• Natural Product Sciences
• /
• 제27권4호
• /
• pp.280-283
• /
• 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.

• Wind and Structures
• /
• 제18권4호
• /
• pp.375-389
• /
• 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.

• ETRI Journal
• /
• 제32권3호
• /
• pp.440-446
• /
• 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.

• 한국산업보건학회지
• /
• 제19권2호
• /
• pp.81-87
• /
• 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.