• Title/Summary/Keyword: 반복성 및 재현성 평가

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Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry (고성능액체크로마토그래피를 이용한 농산물 중 Mandipropamid의 잔류분석법 확립)

  • Kwon, Chan Hyeok;Chang, Moon Ik;Im, Moo Hyeog;Choi, Hoon;Jung, Da I;Lee, Su Chan;Yu, Jin Young;Lee, Young Deuk;Lee, Jong Ok;Hong, Moo Ki
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.518-525
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    • 2008
  • Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.

Error factors and uncertainty measurement for determinations of amino acid in beef bone extract (사골농축액 시료 중에 함유된 아미노산 정량분석에 대한 오차 요인 및 측정불확도 추정)

  • Kim, Young-Jun;Kim, Ji-Young;Jung, Min-Yu;Shin, Young-Jae
    • Analytical Science and Technology
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    • v.26 no.2
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    • pp.125-134
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    • 2013
  • This study was demonstrated to estimate the measurement uncertainty of 23 multiple-component amino acids from beef bone extract by high performance liquid chromatography (HPLC). The sources of measurement uncertainty (i.e. sample weight, final volume, standard weight, purity, standard solution, calibration curve, recovery and repeatability) in associated with the analysis of amino acids were evaluated. The estimation of uncertainty obtained on the GUM (Guide to the expression of uncertainty in measurement) and EURACHEM document with mathematical calculation and statistical analysis. The content of total amino acids from beef bone extract was 36.18 g/100 g and the expanded uncertainty by multiplying coverage factor (k, 2.05~2.36) was 3.81 g/100 g at a 95% confidence level. The major contributors to the measurement uncertainty were identified in the order of recovery and repeatability (25.2%), sample pretreatment (24.5%), calibration-curve (24.0%) and weight of the reference material (10.4%). Therefore, more careful experiments are required in these steps to reduce uncertainties of amino acids analysis with a better personal proficiency improvement.

Estimation of Diagnostic Range for Measurement Tools, while BMD Testing to Health Examination in Transitional Ages (생애전환기 건강진단 골밀도 검사시 측정도구에 따른 진단범위의 유효성 평가)

  • Kim, Nam-Soo;Jung, Kyung-Sick;Kang, Eun-Jung;Oh, Jung-Eun;Lee, Byung-Kook
    • The Journal of the Korea Contents Association
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    • v.12 no.10
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    • pp.385-394
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    • 2012
  • The aim of this study was to determine the effectiveness of diagnostic range for BMD measurement tools(DEXA, QUS, and RA) to health examination in transitional ages. In standard T-score -2.5 of DEXA, cutoff value by RA is -1.675(sensitivity: 70.0%, specificity: 63.7%) and cutoff value by QUS is -1.733(sensitivity: 70.4, specificity: 59.5%), also T-score -3.0 of DEXA, cutoff value by RA is -2.325(sensitivity: 70.0%, specificity: 42.9%) and cutoff value by QUS is -2.323(sensitivity: 70.4, specificity: 56.8%). There was, however, no significant difference in standard DEXA(lumbar spine and femur) between RA and QUS by repeat measurement(precision), and correlation were without effect. ROC analysis showed that all methods are qualified for BMD measurement tools to health examination in transitional ages; however, the different sensitivities and specificities of the methods, as well as age and gender, calibration parameters for diagnostic tests have to be considered.

A development of bivariate regional drought frequency analysis model using copula function (Copula 함수를 이용한 이변량 가뭄 지역빈도해석 모형 개발)

  • Kim, Jin-Guk;Kim, Jin-Young;Ban, Woo-Sik;Kwon, Hyun-Han
    • Journal of Korea Water Resources Association
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    • v.52 no.12
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    • pp.985-999
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    • 2019
  • Over the last decade, droughts have become more severe and frequent in many regions, and several studies have been conducted to explore the recent drought. Copula-based bivariate drought frequency analysis has been widely used to evaluate drought risk in the context of point frequency analysis. However, the relatively significant uncertainties in the parameters are problematic when available data are limited. For this reason, the primary purpose of this study is to develop a regional drought frequency model based on the Copula function. All parameters, including marginal and copula functions in the regional frequency model, were estimated simultaneously. Here, we present a case study of recent drought 2013-2015 over the Han-River watershed where severe drought risk is consistently found to increase. The proposed model provided a reliable way to significantly reduce the uncertainty of parameters with a Bayesian modeling framework. The uncertainty of the joint return period in the regional frequency analysis is nearly three times lower than that of the point frequency analysis. Accordingly, DIC values in the regional frequency analysis model are significantly decreased by 15. The results confirm that the proposed model is not only reliably representing characteristics of historical droughts and dependencies between drought variables, but also providing the efficacy of understanding regional drought characteristics.

Method Development and Validation for Analysis of Isopyrazam Residues in Agricultural Products (농산물 중 살균제 Isopyrazam의 개별 잔류분석법 확립)

  • Kim, Ji-Yoon;Kim, Ja-Young;Ham, Hun-Ju;Do, Jung-Ah;Oh, Jae-Ho;Lee, Young-Deuk;Hur, Jang-Hyun
    • The Korean Journal of Pesticide Science
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    • v.17 no.2
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    • pp.84-93
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    • 2013
  • Validated analytical methods for isopyrazam are meager or lacking. In the present study, a single residual analytical method was developed for isopyrazam in selected commodities. Isopyrazam was analyzed in brown rice, soybean, green pepper, mandarin, cucumber, and Korean melon. We tried different solvents and methods through extraction, partition and purification steps to obtain best analytical results. For isopyrazam samples were extracted with acetonitrile, concentrated and partitioned with n-hexane, clean-up using florisil with n-hexane/ethylacetate (70/30) and analyzed with HPLC/UVD. The limit of quantitation (LOQ) for isopyrazam was 1.0 ng (S/N > 10) and method LOQ (MLOQ) was 0.04 mg $kg^{-1}$. Recovery ranged through 81.0~105.3% (syn-isomer) and 80.8~105.6% (anti-isomer) at fortification level of 0.04 (MLOQ), 0.4 (10 ${\times}$ MLOQ), and 2.0 (50 ${\times}$ MLOQ). The coefficient of variation (CV) for isopyrazam was less than 10% regardless of sample types. These results were further confirmed with LC/MS, respectively. The proposed method is highly reproducible and sensitive and is suitable for routine analysis.

Improvement of Validity and Efficiency for Detection of Cryptosporidium Ocysts and Giardia Cysts in Environmental Water Samples (환경수 중 크립토스포리디움 오시스트 및 지아디아 시스트 검출의 정확도 및 회수율 향상을 위한 연구)

  • 이목영;조은주;김도연;변승헌;이의광;오세종;안승구
    • Korean Journal of Microbiology
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    • v.39 no.1
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    • pp.27-35
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    • 2003
  • No currently available methods to monitor pathogenic protozoa, Cryptosporidium and Giardia in environmental water come close to acceptable sensitivity, specificity and reproducibility, and so it has to be accompanied by thorough quality control and performance evaluation to credibly predict the distribution of them. We collected surface water samples from the Han River and spiked our prepared (oo)cysts, determined Matrix Spike recoveries using USEPA Method 1623 and considered what factors influence MS recovery and validity. As a result, average 46% of spiked oocysts and 60% of spike cysts were recovered, but repetitive sampling and statistical approach seemed to be necessary to determine the environmental pollution level of two protozoa as their variation coefficients was so much as 35oio and 26%. And MS recoveries with two acid dissociations during immunomagnetic separation were improved more 10% than that with one dissociations and the use of spiked suspension enumerated by flow cytometry instead of manual preparation enhanced the validity and reliability in spiking tests. Because fluorescence characteristics of (oo)cysts stained on well slides with FITC-labeled monoclonal antibodies and DAPI was not always same, well Elides from spiked field samples were helpful to evaluate the performance of staining. We found many (oo)cyst-like objects with typical fluorescence, not (co)cysts, from the Han River water samples, and then it was concluded that nuclei staining by DAPI (4',6-diamidino-2-phenylindole) and examination by Differential Interference Contrast Microscope should be critical for valid identification.

A proposal of soft tissue landmarks for craniofacial analysis using three-dimensional laser scan imaging (3차원 레이저 스캔을 이용한 안면 연조직 분석을 위한 계측점의 제안)

  • Baik, Hyoung-Seon;Lee, Hwa-Jin;Jeon, Jai-Min
    • The korean journal of orthodontics
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    • v.36 no.1 s.114
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    • pp.1-13
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    • 2006
  • Three-dimensional (3-D) laser scans can provide a 3-D image of the face and it is efficient in examining specific structures of the craniofacial soft tissues. Due to the increasing concerns with the soft tissues and expansion of the treatment range, a need for 3-D soft tissue analysis has become urgent. Therefore, the purpose of this study was to evaluate the scanning error of the Vivid 900 (Minolta, Tokyo, Japan) 3-D laser scanner and Rapidform program (Inus Technology Inc., Seoul, Korea) and to evaluate the mean error and the magnification percentage of the image obtained from 3-D laser scans. In addition, soft tissue landmarks that are easy to designate and reproduce in 3-D images of normal, Class II and Class III malocclusion patients were obtained. The conclusions are as follows; scanning errors of the Vivid 900 3-D laser scanner using a manikin were 0.16 mm in the X axis, 0.15 mm in the Y axis, and 0.15 mm in the Z axis. In the comparison of actual measurements from the manikin and the 3-D image obtained from the Rapidform program, the mean error was 0.37 mm and the magnification was 0.66%. Except for the right soft tissue gonion from the 3-D image, errors of all soft tissue landmarks were within 2.0 mm. Glabella, soft tissue nasion, endocanthion, exocanthion, pronasale, subnasale, nasal alare, upper lip point, cheilion, lower lip point, soft tissue B point, soft tissue pogonion, soft tissue menton and preaurale had especially small errors. Therefore, the Rapidform program can be considered a clinically efficient tool to produce and measure 3-D images. The soft tissue landmarks proposed above are mostly anatomically important points which are also easily reproducible. These landmarks can be beneficial in 3-D diagnosis and analysis.

Detection of HCV-RNA by Reverse Transcription Polymerase Chain Reaction Using Biotinylated and Radioiodinated Primers (역전사 중합효소 연쇄반응(RT-PCR)에 의한 HCV-RNA의 검출 : Biotin 및 방사성옥소 표지 Primer로 구성된 Kit의 이용)

  • Ryu, Jin-Sook;Moon, Dae-Hyuk;Cheon, Jun-Hong;Chung, Yoon-Young;Park, Hung-Dong;Chung, Young-Hwa;Lee, Young-Sang
    • The Korean Journal of Nuclear Medicine
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    • v.28 no.2
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    • pp.220-226
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    • 1994
  • This study was performed to evaluate the clinical applicability of the reverse transcription polymerase chain reaction (RT-PCR ) kit of HCV-RNA using biotinylated and radioiodinated primers. Study subjects were 118 patients with positive anti-HCV. HCV-RNA in patient's serum was extracted by guanidium thiocyanate method. After first amplification, the product was reamplified by primers labelled with biotin and I-125. The final amplification product was defected by counting the radioactivity after incubation in avidin coated tubes. In 51 samples, the test was repeated for evaluation of reproducibility. This new method was also compared with conventional RT-PCR methods in 34 samples from patients with chronic liver disease. The results were as follows ; 1) HCV-RNA was positive in 85(97%)of 88 patients with chronic liver disease, and in 23 (73%) of 30 patients with normal liver function. 2) In comparison with conventional method, HCV-RNA was detected in 32(94%) of 34 patients with new method, whereas in 27(79%) of the same group with conventional method. 3) Repeated test with new method in 52 samples demonstrated 82% of concordant result. In conclusion, new method with biotinylated and radioiodinated primers was more sensitive than conventional method. However, great care must be taken for quality control because there were considerable interassay variation and possiblity of false positivity and false negativity.

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A development of the Automatic Measuring System for internal pressure of the artillery (화포 내부 압력의 자동 측정시스템 개발)

  • Lee, Jeong-Ho;Kim, Dong-Hee
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.22 no.2
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    • pp.766-773
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    • 2021
  • Chemicals, such as ammunition, are disposable items that cannot be reused because of their operational characteristics. The reliability of the test process and test results are important factors in evaluating the performance of guns and ammunition. The pressure after firing is a crucial value in an acceptance test of guns and ammunition performance; hence, accurate measurements are required. The pressure in the artillery is measured using the copper crusher gauge. The compression amount of copper is converted into a pressure by either a length-pressure conversion table or conversion formula. Therefore, the exact measurement of the squeeze of the copper crusher is related directly to the correct estimate of the pressure. Currently, the pressure is measured manually by the operator, which always includes some human error. In this study, the cause of the measurement error was analyzed, and the automatic measuring system for copper crusher deformation was developed to minimize the error elements. A copper crusher could be measured using the probe sensor and CCD camera, and the Jig for stable positioning was also designed. A designated SW was also developed for the system operating and measurement-analysis. This measuring system through this study may be used for an ammunition stockpile reliability test and gun/ammunition acceptance test.

Development and Validation of an Analytical Method for Fungicide Sedaxane Determination in Agricultural Products using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Sedaxane의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Park, Shin-Min;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.30-39
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    • 2019
  • An analytical method was developed for the determination of sedaxane in agricultural products using liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, and then purified by using silica SPE cartridges to clean up. The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode using multiple reaction monitoring (MRM). The matrix-matched calibration curves were linear over the calibration ranges ($0.001-0.25{\mu}g/mL$) into a blank extract with $r^2$>0.99. For validation, recovery tests were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ, n=5) with five replicates performed at each level. The recoveries were ranged between 74.5 to 100.8% with relative standard deviations (RSDs) of less than 12.1% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for sedaxane determination in agricultural commodities.