• Title/Summary/Keyword: 표준시료

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A Comparative Study on Quantifying Uncertainty of Vitamin A Determination in Infant Formula by HPLC (HPLC에 의한 조제분유 중 비타민 A 함량 분석의 측정불확도 비교산정)

  • Lee, Hong-Min;Kwak, Byung-Man;Ahn, Jang-Hyuk;Jeon, Tae-Hong
    • Korean Journal of Food Science and Technology
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    • v.40 no.2
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    • pp.152-159
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    • 2008
  • The purpose of this study was to determine the accurate quantification of vitamin A in infant formula by comparing two different standard stock solutions as well as various sample weights using high performance liquid chromatography. The sources of uncertainty in measurement, such as sample weight, final smaple vloume, and the instrumental results, were identified and used as parameters to determine the combined standard uncertainty based on GUM(guide to the expression of uncertainty in measurement) and the Draft EURACHEM/CITAC Guide. The uncertainty components in measuring were identified as standard weight, purity, molecular weight, dilution of the standard solution, calibration curve, recovery, reproducibility, sample weight, and final sample volume. Each uncertainty component was evaluated for type A and type B and included to calculate the combined uncertainty. The analytical results and combined standard uncertainties of vitamin A according to the two different methods of stock solution preparation were 627 ${\pm}$ 33 ${\mu}$g R.E./100 g for 1,000 mg/L of stock solution, and 627 ${\pm}$ 49 ${\mu}$g R.E./100 g for 100 mg/L of stock solution. The analytical results and combined standard uncertainties of vitamin A according to the various sample weighs were 622 ${\pm}$ 48 ${\mu}$g R.E./100 g, 627 ${\pm}$ 33 ${\mu}$g R.E./100 g, and 491 ${\pm}$ 23 ${\mu}$g R.E./100 g for 1 g, 2 g, and 5 g of sampling, respectively. These data indicate that the preparation method of standard stock solution and the smaple amount were main sources of uncertainty in the analysis results for vitamin A. Preparing 1,000 mg/L of stock solution for standard material sampling rather than 100 mg, and sampling not more than 2 g of infant formula, would be effective for reducing differences in the results as well as uncertainty.

Validation of Stem-loop RT-qPCR Method on the Pharmacokinetic Analysis of siRNA Therapeutics (Stem-loop RT-qPCR 분석법을 이용한 siRNA 치료제의 생체시료 분석법 검증 및 약물 동태학적 분석)

  • Kim, Hye Jeong;Kim, Taek Min;Kim, Hong Joong;Jung, Hun Soon;Lee, Seung Ho
    • Journal of Life Science
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    • v.29 no.6
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    • pp.653-661
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    • 2019
  • The first small interfering RNA (siRNA) therapeutics have recently been approved by the Food and Drug Administration in the U.S., and the demand for a new RNA therapeutics bioanalysis method-which is essential for pharmacokinetics, including the absorption, distribution, metabolism, and excretion of siRNA therapeutics-is rapidly increasing. The stem-loop real-time qPCR (RT-qPCR) assay is a useful molecular technique for the identification and quantification of small RNA (e.g., micro RNA and siRNA) and can be applied for the bioanalysis of siRNA therapeutics. When the anti-HPV E6/E7 siRNA therapeutic was used in preclinical trials, the established stem-loop RT-qPCR assay was validated. The limit of detection was sensitive up to 10 fM and the lower limit of quantification up to 100 fM. In fact, the reliability of the established test method was further validated in three intra assays. Here, the correlation coefficient of $R^2$>0.99, the slope of -3.10 ~ -3.40, and the recovery rate within ${\pm}20%$ of the siRNA standard curve confirm its excellent robustness. Finally, the circulation profiles of siRNAs were demonstrated in rat serum, and the pharmacokinetic properties of the anti-HPV E6/E7 siRNA therapeutic were characterized using a stem-loop RT-qPCR assay. Therefore, the stemloop RT-qPCR assay enables accurate, precise, and sensitive siRNA duplex quantification and is suitable for the quantification of small RNA therapeutics using small volumes of biological samples.

SNU 1.5-MV 직렬형 반데그라프 가속기를 이용한 러더포드 후방산란 분광법에 의한 소재의 표면적층 분석

  • 박혜일;배영덕;박준교;김명섭;곽종구;김창석
    • Nuclear Engineering and Technology
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    • v.27 no.1
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    • pp.141-153
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    • 1995
  • SNU 1.5-MV 직렬형 반데그라프 가속기로부터 얻은 0.5~2.2 MeV He$^{++}$ 빔을 이용하여 러더포드 후방산란 분광법 (RBS, Rutherford Backscattering Spectrometry)으로 여러가지 시료의 표면적층을 분석하였다. 먼저 RBS 분석계통의 신뢰성을 확인하기 위하여 Micromatter사와 Charles Evans & Associates에서 제작한 14종 33개의 표준시료들에 대한 후방산란 실험을 수행하여, 각 층의 두께, 원소조성비 및 주입 이온의 깊이, 분포폭을 측정하였다. 결정된 이 값들은 제시된 값과 3% 이내로 일치하였다 이와 같이 본 RBS 분석계통의 신뢰성을 확인한 후, 분석을 의뢰받은 22종 87개의 시료에 대해, 빔에너지. 후방산란의 기하학적 구조 등의 최적 조건하에서 후방산란 실험을 수행하였다 그 결과, 분석가능한 두께의 한계를 벗어난 2종 3개의 시료를 제외한 나머지 모든 시료에 대해 각 층의 두께, 원소조성비 및 농도분포를 결정할 수 있었으며, 측정치의 통계오차는 8% 이내였다. 다양한 종류의 많은 시료들에 대한 표면적층 분석을 수행한 경험을 통하여, RBS 분석에서 신뢰도 높은 결과를 얻기 위해 분석계통에서 필수적으로 고려해야 할 요소들을 파악할 수 있었으며, 분석 결과에 대한 신뢰도는 분석 계통의 체계화뿐만 아니라 시료의 상태에 따라 크게 좌우됨을 알 수 있었다. 결론적으로 주의 깊은 시료준비와 RBS 분석계통의 최적화를 통해 신뢰도 높은 표면적층 분석이 가능함을 확인하였다.

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Some Comments on the Preparation of the CSK Standard Chemical Solutions (CSK Standard Chemical Solution 과 그에 대한 몇가지 의견)

  • Won, Chong Hun
    • 한국해양학회지
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    • v.4 no.2
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    • pp.83-86
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    • 1969
  • 해양관측의 세계적인 공통성으로 해서 염분검정법이 이미 오래 전부터 통일화 되었지만 근래에 와서는 용존산소량 정량법도 국제적인 Intercalibration을 하는 등규격화에의 기운이 나고 있다. 다시 Kuroshio 합동조사에서는 영양염의 정량에 있어 공통된 표준용액을 사용하므로써 조작상의 편리와 측정치의 신뢰성을 더욱 향상시키자는 의도에서 일본이 국제적인 영양염 표준용액의 조제 및 배포에 관한 안을 내어 1965년 Manila 회의를 거쳐 일본 상모중앙화학연구소의 관원씨가 이를 맡아 1966년부터 시작하여 1967년까지에 요오드산칼리움, 아질산염, 인산염, 규산염의 표준용액을 만들어 1968년 봄부터 시험적으로 일본국내와 동남아 수개국에 나누어 사용해 왔던 것이다. 다시 1968년 9월의 SCOR 의 영양염에 관한 Working Group 회의에서 CSK Std. Solution을 사용하여 세계각국에서 현재 사용하고 있는 영양염 분석방법의 Intercalibration을 하자는 회의가 있었고, 이것을 권고사항으로 SCOR에 보고하여 1968년 11월에 ICES가 승인하므로써 Intercalibration에 관한 원칙이 정해졌다. 동시에 Finland의 Koroleff씨와 Palmork씨가 organizer로 정해졌던 것이다. 이 보다 약간 앞서 본인이 상모중연에 가 있을 때 Std. Solution으로서 아질산염용액 만으로 각종무기질소화합물의 표준용액으로 대용한다는 것은 비합리적이므로 질산염과 암모늄염의 표준용액이 있어야 한다고 주장하여 우선 질산염용액을 추가로 만들기로 하여 1968년 11월부터 표준물질의 정제부터 시작 되었다. 1969년 1월에 Intercalibration 에 관한 구체적인 회의를 위해 Scripps 해양연구소에 관원, Wooster Rakestraw, Cieskes씨등이 모여 우선 일본상모중연에서 만들고 있는 인산염, 질산염, 아질산염, 규산염의 CSK 표준용액을 표준시료로하여 SCOR 과 ICES의 해양화학분과에서 선정한 세계 100개처에 나누어 현재 각자가 사용하고 있는 방법의 정밀도와 정확도를 check하는 소위 International intercalibration을 1969년 9월부터 시작하기로 확정을 보았고, 동시에 구체적인 지시가 있었던 것이다. 이시료를 받는 사람에게는 다만 그것의 농도범위만 알려주고 정확한 농도는 Koreleff와 관원씨만이 알고 있기로 하여 측정에 분석자의 주관이 개입되지 못하도록 했고, 분석치는 SCOR가 모아 해석하되 번호제로 하여 어떤 나라의 누구가 했다는 것은 밝히지 않기로 되어 있다. 이같은 내력으로 CSK Std. Solution이 국제적인 Intercalibration용의 표준시료로서 시험적으로 사용되기 까지는 되었으나, CSK Std. Solution 그자체에 관해서는 아직도 해결해야 할 점, 개량을 요하는 점이 많다. 이하에서는 주로 개량을 요하는 점에 관해 몇가지 언급하고자 한다.

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Determination of trace boron in steels by prompt gamma-ray activation analysis (즉발감마선방사화분석법에 의한 철강시료 중의 붕소 측정)

  • Kim, I.J.;Cho, K.H.;Paul, R.L.
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.302-306
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    • 2009
  • A trace amount of boron in steel significantly influences its mechanical and physical properties. A prompt gamma ray activation analysis (PGAA) method is used to measure boron in low alloy steel samples of KRISS 101-01-C21~C26. NIST SRMs of 362, 364, 1761 and 1767 serve as the control standards to validate the measurement method. The measured values of the NIST SRMs are consistent with their certified values within the expected uncertainties, except for that of NIST SRM 362. Experimental uncertainties are evaluated according to the guidelines given by the International Organization for Standardization (ISO). The expanded uncertainties are calculated with a coverage factor of 2, at approximately 95% confidence level. The calculated relative expanded uncertainties of boron mass fractions are between 3% and 7% at the mg/kg level. The results are compared with the results measured by the solvent extraction-inductively coupled optical emission spectrometry (ICP/OES) method.

Estimation of Measurement Uncertainty for the HPLC Analysis of Deoxynivalenol in Wheat (밀에서 HPLC에 의한 데옥시니발레놀 분석의 측정불확도 산정)

  • Ok, Hyun-Ee;Chang, Hyun-Joo;Ahn, Jang-Hyuk;Cho, Jae-Young;Chun, Hyang-Sook
    • Korean Journal of Food Science and Technology
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    • v.41 no.3
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    • pp.258-264
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    • 2009
  • The principal objective of this study was to estimate the measurement uncertainty associated with determination of deoxynivalenol (DON), a mycotoxin generated by Fusarium strain, in food. In service of this goal, wheat as a food matrix was analyzed via high performance liquid chromatography-ultraviolet (HPLC-UV) detection using an immunoaffinity column for clean-up. The uncertainty sources in the measurement process were identified by sample weight, final volume, and sample concentration in extraction volume with components including standard stock solution, working standard solution, 5 standard solutions, calibration curve, matrix, and instrument. The expanded uncertainty for DON at a concentration of 300 ${\mu}g/kg$ was estimated as 71.62 ${\mu}g/kg$ using a coverage factor of two, which provides a confidence level of approximately 95%. The most influential component in the uncertainty sources was the recovery of the wheat matrix, followed by the calibration curve. These results indicate that all efforts may be directed toward reducing the uncertainties of the recovery of the wheat matrix and the calibration curve to obtain a reliable HPLC-UV method for DON analysis in wheat.

New Joint Roughness Coefficient and Shear Strength Criterion Based on Experimental Verification of Standard Roughness Profile (표준 거칠기 단면의 실험적 검증에 의한 새로운 거칠기 계수 및 전단강도 기준식)

  • Jang, Hyun-Sic;Sim, Min-Yong;Jang, Bo-An
    • The Journal of Engineering Geology
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    • v.31 no.4
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    • pp.561-577
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    • 2021
  • The ten standard roughness profiles suggested by Barton and Choubey (1977) were extended to make three-dimensional (3D) joint models whose profiles were identical at any cross section. Replicas of joint models were produced using plaster of Paris, and direct shear tests were performed to verify the joint roughness coefficients (JRC) of the standard roughness profiles. Joint shear strengths measured by direct shear tests were compared with those predicted by the shear failure criterion suggested by Barton (1973) based on JRC, joint compressive strength (JCS), and joint basic friction angle (𝜙b). Shear strengths measured from joints of the first and fourth standard roughness profiles were close to predicted values; however, shear strengths measured from the other joint models were lower than predicted, the differences increasing as the roughness of joints increased. Back calculated values for JRC, JCS, and from the results of the direct shear tests show measured shear strengths were lower than predicted shear strengths because of the JRC values. New JRC were back calculated from the measured shear strength and named JRCm. Values of JRCm were lower than the JRC for the standard roughness profiles but show a strong linear relationship to JRC. Corrected JRCm values for the standard roughness profiles are provided and revised relationships between JRCm and JRC, and new shear strength criterion are suggested.

Production of Standard Sample for Quality Control of Total Coliform (총대장균군 측정의 정도관리에 적합한 균주의 조제)

  • Kim, Ju-Young;Seo, Eun-Young;Kim, Mi-Ree;Jeon, Nam-Hui;Chung, Hyen-Mi;Kim, Myeong-Woon;Ahn, Tea-Seok
    • Korean Journal of Microbiology
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    • v.44 no.1
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    • pp.43-48
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    • 2008
  • Standard sample for quality control of total coliform measurement was procured by addition of nalidixic acid and cephalexin as bacteriostatic agents to Escherichia coli cultured broth. After making the standard sample, the number of E. coli was measured by fluorescence microscopic count method and plate count method by 12 hr interval. The numbers of E. coli remained unchanged for at least for 48 hr at room temperature which ranged from 3.5 to $4.2{\times}10^5\;cells/ml$ and from 1.0 to $1.2{\times}10^4\;CFU/ml$ by direct fluorescence microscopic count method and plate count method, respectively. This result suggests that microbial standard sample with bacteriostatic agents of nalidixic acid and cephalexin is usable for quantitative quality control.

The Study of Fast X-ray Fluorescence Analysis Using a SSQ Program (SSQ 프로그램을 이용한 빠른 X-선형광분석법 고찰)

  • Park, Yong Joon
    • Analytical Science and Technology
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    • v.11 no.2
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    • pp.112-119
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    • 1998
  • A Siemens SemiQuant (SSQ) 3000 program, a precalibrated 'standardless' analytical program handling up to 90 elements, was evaluated for the fast analysis of various types of reference materials using a wavelength dispersive X-ray spectrometer. Various types of standard reference materials such as metal discs, metal chips, and geological materials in powder form were analysed and it took 23 minutes of measuring time for 75 elements. Measurements of geological reference materials using different sampling methods were carried out and their data were interactively evaluated. The analysis of materials of a known matrix concentration such as stainless steels provided higher precision value compared to totally unknown samples. The analyses of materials prepared as pressed pellets or fused glass beads provided higher precision values compared to the measurement of loose powders with a foil on the sample surface and helium operation, though their sampling procedures were more complicate and took more time. Since very light elements such as boron, carbon, and oxygen have a strong influence on the matrix effects and also on the calculation of effective matrix corrections, the rhodium Compton check was applied to verify the reliability of the defined light element concentrations of light matrix materials and the defined major sample compounds. Failure of defining correct matrix resulted in an unoptimized matrix correction and therefore in the wrong calculation of the element concentration.

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Quality of Licorice (Glycyrrhiza uralensis) Powder Added Kimchi (감초분말첨가 김치의 품질)

  • Ko, Young-Tae;Lee, Ju-Youn
    • Korean Journal of Food Science and Technology
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    • v.38 no.1
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    • pp.143-146
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    • 2006
  • Effects of licorice (Glycyrrhiza uralensis) powder as sugar substitute on kimchi quality was evaluated by investigating acid formation, lactic acid bacteria growth, and sensory properties of licorice powder added kimchi. Initial pH of licorice powder added kimchi unripened and ripened for one day did not differ from those of other samples, but slightly increased thereafter 2-3 days ripening. Acidities of unripened and kimchi ripened for 1 day significantly increased by addition of licorice powder, while that of kimchi ripened for 2-3 days significantly decreased (p<0.05). Addition of licorice powder had no significant effect on lactic acid bacteria count of kimchi compared to sugar. Overall acceptability and taste of 0.1 and 0.2% licorice powder-added kimchi ripened for 1-3 days were similar to or slightly higher than those of reference sample, whereas addition of 1.0% licorice powder resulted in lowest overall acceptability, taste, odor, and texture. Licorice powder addition generally did not change color of kimchi.