• 제목/요약/키워드: method validation #5

검색결과 959건 처리시간 0.032초

인체 혈장 중 칼시트리올의 효소면역 분석법 검증 및 단회투여 후 약물동태 연구 (Validation of an Enzyme-Immunoassay for Calcitriol in Human Plasma and Evaluation of Its Pharmacokinetics after Single-dose in Korean Volunteers)

  • 김예태;진수언;김현기;신백기;정의현;김종국;박정숙
    • Journal of Pharmaceutical Investigation
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    • 제39권4호
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    • pp.309-314
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    • 2009
  • An enzyme immunoassay (EIA) was validated for quantitation of cacitriol in human plasma. Calcitriol was immunoextracted with immunocapsules, which contain monoclonal antibodies to calcitriol linked to solid phase particles in suspension with a vitamin D binding protein inhibitor. Calcitrol was eluated and the eluates were evaporated under a gentle stream of nitrogen gas. The absorbance of analytes was determined using a microplate reader (reference wavelength 650 nm; measurement wavelength 450 nm). The method was specific and sensitive enough to detect as low as 6.5 pmol/L of calcitriol. Linear calibration range was 6.5-491 pmol/L with correlation coefficient greater than 0.99. The overall accuracy was in the range of 83.8 to 111.2% and precision C.V. (%) 0.99 to 8.47%. The recovery was approximately 100% and stability was confirmed during storage and sample preparation. The pharmacokinetic parameters were calculated by baseline subtraction because calcitriol is an endogenous material. Following oral dose of calcitriol, the mean AUC$_{24h}$ was 1038${\pm}$539 pmol/Lhr and C$_{max}$ of 128${\pm}$63.1 pmol/L was reached at 3.50${\pm}$1.07 hr. The mean t$_{1/2}$ of calcitriol was 5.13${\pm}$2.10 hr. The present EIA method was successfully applied to study bioavailability after oral administration of 2 ${\mu}$g of calcitriol in healthy Korean subjects.

DACUM 기법에 의한 영양교사 직무기술서 개발 (Development of Job Description of Nutrition Teacher by the DACUM Method)

  • 김지희;차진아
    • 대한영양사협회학술지
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    • 제22권3호
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    • pp.193-213
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    • 2016
  • The purpose of this study is to provide a standard job description for a nutrition teacher placed in primary and secondary schools by analyzing their duties. DACUM is an acronym for 'Developing A CUrriculuM'. It was used by experts to determine the job duties, tasks and task elements to establish the job descriptions of a nutrition teachers through the development of a DACUM chart. An expert panel consisting of 10 nutrition teachers participated in a DACUM workshop and derived nutrition teacher's DACUM chart. A total of 1,550 nutrition teachers across the country were targeted as the survey subjects for validation of the DACUM chart through their perception of the frequency, importance, and difficulty of each item in the job description. A tree structure, criticality analysis, and contents validity index were added for verification. The definition of the nutrition teacher's job and DACUM chart with 5 duties, 28 tasks, and 107 task elements were derived by the DACUM method. The definition of a nutrition teacher was 'A teacher who is responsible for food service management and nutrition education and counseling for health promotion and disease prevention for students in primary and secondary schools'. The validation results of the tree structure were the priorities of the 28 tasks with ranks 1 and 2. Because there was no third priority, it was considered to be a good representation of the tasks of nutrition teachers. The DACUM chart was found to be evenly distributed with relative importances of more than 17 or less than 11 through the criticality analysis. Since the C5-4 (Conduct simulation exercise against food poisoning)'s content validity index was significantly less than the reference value of 0.78, it was not included in the final job description. 5 duties, 28 tasks, 102 task elements were included in the final job description of a nutrition teacher.

Improved first-order method for estimating extreme wind pressure considering directionality for non-typhoon climates

  • Wang, Jingcheng;Quan, Yong;Gu, Ming
    • Wind and Structures
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    • 제31권5호
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    • pp.473-482
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    • 2020
  • The first-order method for estimating the extreme wind pressure on building envelopes with consideration of the directionality of wind speed and wind pressure is improved to enhance its computational efficiency. In this improved method, the result is obtained directly from the empirical distribution of a random selection of annual maximum wind pressure samples generated by a Monte Carlo method, rather than from the previously utilized extreme wind pressure probability distribution. A discussion of the relationship between the first- and full-order methods indicates that when extreme wind pressures in a non-typhoon climate with a high return period are estimated with consideration of directionality, using the relatively simple first-order method instead of the computationally intensive full-order method is reasonable. The validation of this reasonableness is equivalent to validating two assumptions to improve its computational efficiency: 1) The result obtained by the full-order method is conservative when the extreme wind pressure events among different sectors are independent. 2) The result obtained by the first-order method for a high return period is not significantly affected when the extreme wind speeds among the different sectors are assumed to be independent. These two assumptions are validated by examples in different regions and theoretical derivation.

간장 및 이를 활용한 식품의 레불린산 분석방법 검증 및 모니터링 (Analytical method validation and monitoring of levulinic acid in soy sauce and their application to food)

  • 김단비;김선영;이상희;유미영
    • 분석과학
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    • 제30권5호
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    • pp.295-302
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    • 2017
  • 본 연구는 High liquid chromatograph-photodiode array detector (HPLC-PDA)를 사용하여 간장 및 이를 활용한 식품에서의 레불린산을 측정하기 위하여 신속 정확한 분석법을 개발하였다. 시료 중 레불린산은 증류수로 추출한 후 C18 Sep-Pak 카트리지로 정제하여 기기분석을 수행하였다. 직선성은 비교적 넓은 농도 범위 ($2.5-400{\mu}g/mL$)에서 우수한 선형성 (R > 0.999)을 나타내었으며, 간장 시료에 대하여 레불린산의 회수율을 확인한 결과, 6 가지 농도범위($2.5-400{\mu}g/mL$)에서 87.58-97.26 %로 확인되었으며, 모두 15 % 미만의 표준오차를 나타내었다. 검출한계(LOD)와 정량한계(LOQ)는 각각 0.64와 $1.64{\mu}g/mL$이었다. 간장 및 이를 활용한 식품에서의 레불린산 함량을 조사한 결과 59 개의 샘플 중 43 개의 샘플에서 검출되었다. 검출 수준은 간장의 경우 0.44-1.23 mg/mL, 간장 소스의 경우 0.03-0.83 mg/mL, 양념육의 경우 8.43-38.94 mg/mL로 나타났다. 따라서 본 연구에서 개발된 분석법은 신속하고 정확하게 레불린산을 정량하고 간장 및 이를 활용한 상품의 적절한 품질 관리 방법으로 사용될 것으로 판단된다.

식품 색소 Canthaxanthin의 HPLC 최적 분석법 확인 및 타당성과 측정불확도 평가 (Validation and Uncertainty Evaluation of an Optimized Analytical Method Using HPLC Applied to Canthaxanthin, a Food Colorant)

  • 서희재;김경수;홍미나;이찬
    • 한국식품영양과학회지
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    • 제45권3호
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    • pp.342-351
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    • 2016
  • 본 연구는 한국에서 식용색소로 지정되지 않은 keto-carotenoid계의 canthaxanthin에 대한 최적 분석방법을 확보하기 위해 수행되었다. HPLC-UVD를 이용한 외국의 canthaxanthin 공인분석법을 검토하여 직선성, 분리능, 민감도, 검출한계(LOD), 정랑한계(LOQ)를 도출하고, 각 실험 데이터를 비교하여 최적의 canthaxanthin 분석방법을 확보하였다. 또한 확보된 최적 분석방법에 대한 정밀도, 정확도, 회수율, 실험실 간 교차검증, 측정불확도를 산출하여 canthaxanthin 최적 분석법에 대한 타당성을 검증하였다. AOAC법, 일본 및 영국의 공인분석법을 이용하여 canthaxanthin 표준용액을 5, 10, 20, 50, 100, $300{\mu}g/mL$의 6 point로 희석한 후 얻은 검량선의 상관계수는 모두 $R^2=0.999$ 이상으로 나타나 우수한 직선성을 보였으나 분리능, 민감도, LOD, LOQ는 일본의 공인분석법이 가장 우수하였다. 일본 공인분석법의 LOD와 LOQ는 각각 0.084 mg/kg, 0.254 mg/kg으로 나타났으며, 1보다 낮은 정밀도, 100%에 가까운 정확도, $100{\pm}10%$ 사이의 회수율, 교차검증 시 세 기관의 변동계수가 5이하로 나타나 canthaxanthin 분석을 위해 가장 최적화된 방법으로 확인되었다. 또한 측정하는 중에 나타나는 불확실성을 알아보기 위하여 canthaxanthin이 함유된 가공식품을 분석하여 측정불확도를 산출한 결과 $39.5{\pm}5.29mg/kg$(95% 신뢰구간, k=2.78)으로 나타났다. 확장불확도는 측정 농도의 13.4%로 나타나 유럽연합의 기준(16% 이하)에 적합한 결과를 보였다.

무인차량 자율주행을 위한 레이다 영상의 정지물체 너비추정 기법 (Width Estimation of Stationary Objects using Radar Image for Autonomous Driving of Unmanned Ground Vehicles)

  • 김성준;양동원;김수진;정영헌
    • 한국군사과학기술학회지
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    • 제18권6호
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    • pp.711-720
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    • 2015
  • Recently many studies of Radar systems mounted on ground vehicles for autonomous driving, SLAM (Simultaneous localization and mapping) and collision avoidance have been reported. Since several pixels per an object may be generated in a close-range radar application, a width of an object can be estimated automatically by various signal processing techniques. In this paper, we tried to attempt to develop an algorithm to estimate obstacle width using Radar images. The proposed method consists of 5 steps - 1) background clutter reduction, 2) local peak pixel detection, 3) region growing, 4) contour extraction and 5)width calculation. For the performance validation of our method, we performed the test width estimation using a real data of two cars acquired by commercial radar system - I200 manufactured by Navtech. As a result, we verified that the proposed method can estimate the widths of targets.

대체용매를 이용한 금속가공유 측정방법 타당성 평가 (Validation of an Extraction Method for the Determination of Airborne MWFs using Alternative Solvents)

  • 정지연;백남원
    • 한국산업보건학회지
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    • 제16권2호
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    • pp.91-100
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    • 2006
  • The purpose of this study was to validate alternative method by using non-carcinogenic, and less toxic solvents than NIOSH analytical method 5524 for measuring the airborne MWFs in workplaces. In laboratory tests, the ETM solvents(mixture of same volume for ethyl ether, toluene, and ethanol) were selected. The alternative method of analyzing MWFs, referred to as the ETM solvent extraction method, showed 0.04 mg/sample as LOD, and 0.15 mg/sample as LOQ. The analytical precision (pooled CV, coefficient of variation) of the ETM solvent extraction method for analyzing the straight, soluble, semisynthetic, and synthetic metalworking fluid was 1.5%, 2.0%, 2.6%, 1.6%, respectively, which was similar to the precision (2.6%) of NIOSH analytical method (NIOSH 0500) for total dust. The analytical accuracy by recovery test, spiked mass calculated as extractable mass, was almost 100%. As the result of storage stability test, metalworking fluid samples should be stored in refrigerated condition, and be analyzed in two weeks after sampling. The 95% confidence limit of the estimated total standard error for the ETM solvent extraction method for analyzing the straight, soluble, semisynthetic, and synthetic metalworking fluid was ${\pm}12.6%$, ${\pm}12.5%$, ${\pm}14.0%$, and ${\pm}13.6%$, respectively, which satisfied the OSHA sampling and analytical criteria.

성충동약물치료 시행에 따른 소변 중 남성호르몬의 분석법 확립 (Validation of Analytical Method for Male Sex Hormone Monitoring in Urine due to the Chemical Castration)

  • 정수진;백승경;박선혜;손꽃잎;박용훈;이상기
    • 약학회지
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    • 제57권5호
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    • pp.330-336
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    • 2013
  • "The Act on Medication Treatment of Sexual Impulse of Sex Offenders" known as chemical castration has been effective since July 2011 in Korea. According to the law, monitoring of male sex hormone in urine is enforced to request National Forensic Service more than once a month after injection of medicine designed to reduce sex impulse. We established a rapid and sensitive method for the monitoring of testosterone (T) and epitestosterone (E) in human urine by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Three mL of urine was pretreated by solid-phase extraction for purification and performed enzymatic hydrolysis. The pretreated samples were extracted twice with 2 ml of ethyl acetate and n-hexane (2 : 3). The separation was applied on Thermo Hypersil GOLD C18 column ($1.9{\mu}m$, $100{\times}2.1mm$). A gradient elution of methanol and water of 0.1% formic acid were used as mobile phase and the retention time was less than 10 min. LC-MS/MS system coupled with an electrospray ionization source was performed in multiple reaction monitoring mode. The transitions of the analytes executed as following: m/z $289{\rightarrow}97$, 109 for T and E, m/z $292{\rightarrow}109$ for $T-d_3$ and $E-d_3$ as internal standards. The validation results of the method were satisfactory. The limits of detection were 0.05 ng/ml and the limits of quantification were 0.1 ng/ml. This method was successfully applied to real human urine sample. The developed method will be useful for monitoring T/E ratio in urine of sex offenders.

THE SIMPLE METHOD OF GEOMETRIC RECONSTRUCTION FOR SPOT IMAGES

  • JUNG HYUNG-SUP;KIM SANG-WAN;WON JOONG-SUN
    • 대한원격탐사학회:학술대회논문집
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    • 대한원격탐사학회 2004년도 Proceedings of ISRS 2004
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    • pp.205-207
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    • 2004
  • The simple method of the geometric reconstruction of satellite linear pushbroom images is investigated. The model of the sensor used is based on the SPOT model that is developed by Kraiky. The satellite trajectory is a Keplerian trajectory in the approximation. Four orbital parameters, longitude of the ascending $node(\omega),$ inclination of the orbit plan(I), latitude argument of the satellite(W) and distance between earth center and satellite, are used for the camera modeling. We suppose that four orbital parameters and satellite attitude angles are exactly acquired. Then, in order to refine model, the given attitude angles and orbital parameters is not changed, but time-independent four parameters associated with LOS(Line Of Sight) vector is updated. A pair of SPOT-5 images has been used for validation of proposed method. Two GCPs acquired by GPS survey is used to controlling the LOS vector. The results are that the RMSE of 16 checking points are about 4.5m. Because the ground resolution of SPOT-5 is 2.5m, the result obtained in this study has a good accuracy. It demonstrates that the sensor model developed by this study can be used to reconstruct the geometry of satellite image taken by pushbroom camera.

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Optimization of the Lowry Method of Protein Precipitation from the H. influenzae Type b Conjugate Vaccine Using Deoxycholic Acid and Hydrochloric Acid

  • Kim, Hyun-Sung;Kim, Sang-Joon;Kim, Hui-Jung;Kim, Han-Uk;Ahn, Sang-Joem;Hur, Byung-Ki
    • Biotechnology and Bioprocess Engineering:BBE
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    • 제11권3호
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    • pp.215-222
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    • 2006
  • The Lowry method was used in this study to measure protein in Haemophilus influenzae type b (Hib) conjugate vaccines (polyribosylibitol phosphate-tetanus toxoid; PRP-TT) using deoxycholic acid (DOC) to induce protein precipitation. Trichloroacetic acid (TCA) did not induce precipitation adequately from the Hib conjugate bulk and the freeze-dried Hib conjugate product. Its yield was approximately 50%. The matrix structure of Hib conjugate inhibits precipitation by TCA. Although the Lowry method can be carried out without precipitation in Hib conjugate bulk when no residual impurities (adipic acid dihydrazide [ADH], 1-ethyl-3-(3-dimethylamino-propyl) carbodiimide-HCI [EDAC], phenol and cyanogens bromide [CNBr], etc.) are present, it cannot be used for Hib conjugate products that contain sucrose 8.5%, because 8.5% concentration of sucrose enhanced the protein concentration. DOC- and HCl-induced precipitation is an alternative method for evaluating the protein content of the Hib conjugate bulk and the Hib conjugate product. The precipitation was optimal with a final concentrate of 0.1% for DOC at $4^{\circ}C$ and pH 2. This Lowry method, using DOC/HCI precipitation to induce protein precipitation, was confirmed a consistent, reproducible, and valid test for proteins in Hib conjugate bulk and its freeze-dried product.