• Title/Summary/Keyword: Standard reference material

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Development of Isotope Dilution LC-MS/MS Method for Accurate Determination of Arsenobetaine in Oyster Certified Reference Material

  • Lee, Woo Young;Yim, Yong-Hyeon;Hwang, Euijin;Lim, Youngran;Kim, Tae Kyu;Lee, Kyoung-Seok
    • Bulletin of the Korean Chemical Society
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    • v.35 no.3
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    • pp.821-827
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    • 2014
  • An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, ${(CH_3)_3}^+AsCH_2COO^-$) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using $^{13}C_2$-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as $6.60mg{\cdot}kg^{-1}{\pm}0.31mg{\cdot}kg^{-1}$ and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.

Analysis of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol in urine with certified reference material (인증표준물질(CRM)을 이용한 소변 중 대마 대사체 분석법 평가)

  • Ko, Beom-Jun;Kim, Jin-Young;Kim, Jong-Sang;Lee, Jeong-Jik;Cheong, Jae-Chul;Suh, Sung-Ill;In, Moon-Kyo
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.83-88
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    • 2010
  • For the evaluation of our laboratory's 11-nor-${\Delta}^9$-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) urinalysis test, THCCOOH urinalysis test was carried out with Certified Reference Material (CRM). The used CRM was THCCOOH in freeze-dried urine produced by NIST as Standard Reference Material 1507b. Comparing the estimated value of our laboratory with CRM, the results was coincided in the confidence level of approximately 95%.

Development of Analytical Reference Material for Proficiency Test of Pesticide Multi-residue Analysis in Tomato (토마토 농약다성분분석 정도관리용 분석표준물질 개발)

  • Kim, Jong-Hwan;Oh, Young-Gon;Choi, Sung-Gil;Hong, Su-Myeong;Kim, Sun-bae;Woo, In-Duk;Kim, Jun-Young;Seo, Jong-Su
    • Korean Journal of Environmental Agriculture
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    • v.35 no.3
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    • pp.223-233
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    • 2016
  • BACKGROUND: This study was to develop a analytical reference material including twenty pesticides in tomato. To use it for proficiency test, the suitability of homogeneity, storage stability, assigned values and uncertainty for analytical reference material were important.METHODS AND RESULTS: In order to develop a analytical reference material of tomato for multi-residue analysis of pesticides, twenty-pesticides were treated in tomato and the samples were frozen and homogenized. The homogeneity, stability, assigned value and uncertainty were calculated according to the requirements of the KS A ISO Guide 35, KS Q ISO 13528 and EURL-PT protocol. The values of the within-bottle standard variation(swb) and the between-bottle standard variation(sbb) were 0.9~6.5% of assigned value and the uncertainty(u*bb) due to inhomogeneity was also calculated as 0.6~1.9% for all pesticides. This indicated that it was satisfactory to be used as a analytical reference material. The storage stabilities of twenty-pesticides at room temperature and freezing conditions were assessed according to the requirement of the KS Q ISO Guide 35. All pesticides were stable at room temperature (20~30℃) for 8 days and freezing (-20℃) for 23 days.CONCLUSION: The feasibility of analytical reference material for pesticide multi-residue analysis in a tomato matrix was investigated. Homogeneity of within/between-bottle, uncertainty and stabilities at room temperature and freezing condition were satisfactory for a use of proficiency test and quality control. From these results, a analytical reference material would be applicable to monitor the proficiency test of pesticide analysis organizations to improve the reliability and consistency.

The Evaluation of Recovery Rate of Radioimmunoassay Using Certified Reference Material (CRM) (인증표준물질(CRM)을 이용한 방사면역측정법의 회수율 평가)

  • Choi, Sung Hee;Shin, Sun Young;Lim, So Hee;Hong, Mee Kyung;Noh, Gyeong Woon;Kim, Jin Eui
    • The Korean Journal of Nuclear Medicine Technology
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    • v.18 no.1
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    • pp.158-162
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    • 2014
  • Purpose: Reference material (RM) is defined as material that is safe and homogeneous enough about specified characteristic that is made with a purpose of using test of measurement or nominal characteristic. Certified reference material (CRM), which is issued by authorized organization, is defined as reference material that provides characteristic value, link uncertainty and retroactivity. The purpose of this paper was to evaluate recovery of radioimmunoassay by Certified Reference Material enclosed with a certificate and therefore to enhance reliability of test. Materials and Methods: WHO certified reference material is purchased from NIBSC (National Institute for Biological Standard and Control, United Kingdom) and made of 3 levels that are C-1 (low concentration), C-2 (medium concentration) and C-3 (high concentration) and measured for kit at the Seoul National University Hospital. Recovery rate is evaluated after measurement at four different days. Results: Recovery rate results using WHO certified reference material are T4 90%, Ferritin 88%, PSA 94%, Prolactin 99%, AFP 94% and TSH 93%. Conclusion: A procedure that appropriate accuracy, precision, specificity, sensitivity, reproducibility, and validate on the subject of kit for radioimmunoassay is essential. Recovery rate assay as extraction efficiency of analysis process is percent about already measuring results of analysis result after all measuring process. This is very important assessment standards of performance evaluation of immunoassay kit. Recovery rate results of 6 type used WHO CRM are satisfactory to 88~99%. This demonstrates that the radioimmunoassay is a very accurate measurement, which is very effectively utilized in clinical practice.

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Development of a Nutritional Supplement Certified Reference Material for Elemental Analysis

  • Lee, Jong Wha;Heo, Sung Woo;Kim, Hwijin;Lim, Youngran;Lee, Kyoung-Seok;Yim, Yong-Hyeon
    • Mass Spectrometry Letters
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    • v.9 no.4
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    • pp.105-109
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    • 2018
  • A certified reference material (CRM) for the analysis of inorganic nutrients in nutritional supplements has been developed. Accurate mass fractions of chromium (Cr), iron (Fe), copper (Cu), and zinc (Zn) were determined by isotope dilution inductively coupled plasma mass spectrometry (ID ICP/MS). The measurement results were used to assign certified values for the CRM, which were metrologically traceable to the definitions of the measurement units in the International System of Units (SI). Production of a candidate reference material (RM) and the certification processes are summarized. Each nutrient in the CRM showed good homogeneity, which was estimated using relative standard deviations of the measurement results of twelve bottles in a batch. This CRM is expected to be an important reference to improve reliability and comparability of nutrient analyses in nutritional supplements and related samples in analytical laboratories.

Development of a Chloroform Reference Material for the Proficiency Testing of Hazardous Compounds in Commercial Consumer Chemical Products Under the Consumer Chemical Products and Biocide Safety Management Act (K-BPR)

  • Lee, Sang Tak;Lee, Jae-ung;Kim, Joo-Hyon;Oh, Han Bin
    • Mass Spectrometry Letters
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    • v.10 no.4
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    • pp.112-116
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    • 2019
  • In this study, a chloroform consumer chemical product (CCP) reference material (RM) is successfully developed, with potential to be used in the proficiency testing of hazardous compounds in CCPs for analysis and testing agencies. Validation experiments are rigorously conducted to evaluate whether the RM meets the requirements set by the ISO 13528 and ISO Guide 35, using a reliable GC/MS method for the analysis of chloroform. The obtained calibration plot linearity, limit of detection (LOD), and limit of quantitation (LOQ) are excellent. The developed RM meets the homogeneity and stability requirements; the between-unit (sbb) and within-unit (swb) standard deviations are less than 2.5%, and the stability is found to be guaranteed for 50 days.

Nondestructive Prediction of Fatty Acid Composition in Sesame Seeds by Near Infrared Reflectance Spectroscopy

  • Kim, Kwan-Su;Park, Si-Hyung;Choung, Myoung-Gun;Kim, Sun-Lim
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.51 no.spc1
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    • pp.304-309
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    • 2006
  • Near infrared reflectance spectroscopy (NIRS) was used to develop a rapid and nondestructive method for the determination of fatty acid composition in sesame (Sesamum indicum L.) seed oil. A total of ninety-three samples of intact seeds were scanned in the reflectance mode of a scanning monochromator, and reference values for fatty acid composition were measured by gas-liquid chromatography. Calibration equations were developed using modified partial least square regression with internal cross validation (n=63). The equations obtained had low standard errors of cross-validation and moderate $R^2$ (coefficient of determination in calibration). Prediction of an external validation set (n=30) showed significant correlation between reference values and NIRS estimated values based on the SEP (standard error of prediction), $r^2$ (coefficient of determination in prediction) and the ratio of standard deviation (SD) of reference data to SEP. The models developed in this study had relatively higher values (more than 2.0) of SD/SEP(C) for oleic and linoleic acid, having good correlation between reference and NIRS estimate. The results indicated that NIRS, a nondestructive screening method could be used to rapidly determine fatty acid composition in sesame seeds in the breeding programs for high quality sesame oil.

A Study on the Quality Control and Operating System of Standard Reference Data(SRD) (참조표준데이터 품질관리 및 운영체계에 관한 연구)

  • Chae Kyun-shik;Lee Eung-Bong
    • Journal of Korean Library and Information Science Society
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    • v.36 no.2
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    • pp.283-305
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    • 2005
  • Data produced during scientific and technical activities usually have value as standard reference data (SRD) which is a well-documented numeric value assessed for reliability and accuracy. The main criteria in the evaluation for SRD is how well their production is documented including a sample preparation, measurement method, data processing and so on, other than reference data. SRD is represented as a certified numeric value with uncertainty. In this study, the SRD in the area of material properties was introduced to provide understanding of SRD and its evaluation method. Also the national SRD system was studied. The national SRD system is composed of the center for the SRD, the data centers, and the committee. The role and task of those components were studied. The legislational and systematic supports for the system were proposed in this study.

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Development of Certified Reference Materials for Analysis of Heavy Metals in Paints to Cope with Environmental Regulations (환경규제 대응을 위한 페인트 중의 중금속 분석용 인증 표준물질 개발)

  • Yu, Byung Kyu;Sun, Yle Shik
    • Journal of Environmental Analysis, Health and Toxicology
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    • v.21 no.4
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    • pp.209-219
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    • 2018
  • In the areas of RoHS, WEEE, ELV and REACH, reinforcement of environmental regulations against harmful substances is a global trend not only in EC but also in all over the world. In the fields of Korea's major export products such as material parts, electrical and electronic products and automobile parts, we are responding to these regulations consistently. To develop reference material for analyzing lead and cadmium in paints, the candidate materials were produced through the screening process which separated shapes and sizes. To secure the traceability of the candidate materials produced, the characteristics and uncertainties are estimated by ICP-AES analysis using the primary reference material. The short-term and long-term stabilities also are evaluated in parallel. In order to calculate the final certification value of the candidate material, the verification were carried out by the performance evaluation through the comparison among the KOLAS (Korea Laboratory Accreditation Scheme) laboratories, and the CRM was produced in accordance with ISO Guide 35. The certified values and uncertainties of Pb and Cd of the final paint standard, determined according to the joint analysis among laboratories, are Pb [($191.4{\pm}3.1$) mg/kg, ($944.1{\pm}5.6$) mg/kg] and Cd [($45.0{\pm}2.6$) mg/kg, ($225.5{\pm}3.5$) mg/kg]. These standard materials were developed to enhance the reliability of measurement analysis, including the validity and traceability of measurement results. Also it is expected that the CRM will be used as QCM (quality control material) for the product design and the process monitoring, so that regulation and management of hazardous heavy metals can be systematically implemented.

RRT Study for the Quantitative Analysis of Boron in Silicon (실리콘에 도핑된 붕소의 정량분석에 대한 공동분석연구)

  • 김경중;김현경;문대원;홍태은;정칠성;김이경;김재남;임철호;김정호
    • Journal of the Korean Vacuum Society
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    • v.11 no.4
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    • pp.218-224
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    • 2002
  • A domestic round robin test(RRT) for the quantitative analysis of minor impurities was performed by a standard procedure and standard reference material. The certified reference material(CRM)s for B-doped Si thin film and analysis specimens and the analysis specimens were prepared by an ion beam sputter deposition method. These samples were certified by inductively coupled plasma mass spectrometry(ICP-MS) with isotope dilution method which il one of the most quantitative methods in chemical analysis. By using an international standard procedure(ISO/DIS-l4237) for the quantitative analysis of B in Si by SIMS, a domestic RRT was performed for these specimens. Although only a few laboratories participated in this RRT, the average B concentration well agreed with the certified value within 2% error.