• Bulletin of the Korean Chemical Society
• /
• 제35권3호
• /
• pp.821-827
• /
• 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.

• 분석과학
• /
• 제23권1호
• /
• pp.83-88
• /
• 2010

대검찰청 마약감식실은 대마 흡연여부를 판별하는 수단인 소변 중 대마 대사체 성분 분석법 에 대한 신뢰도 평가를 위하여 인증표준물질을 이용한 시험을 실시하였다. 시험에 사용된 인증표준물질은 미국 NIST에서 판매하는 Standard Reference Material 1507b로, 11-nor-${\Delta}^9$-tetrahydrocannabinol-9-carboxylic acid (THCCOOH)가 함유된 냉동 건조 소변이었다. NIST에서 구매한 인증표준물질의 농도값과 실험실에서 측정한 농도값을 비교 평가해 본 결과, 약 95% 신뢰수준에서 일치하였다.

• 한국환경농학회지
• /
• 제35권3호
• /
• pp.223-233
• /
• 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(s_wb) and the between-bottle standard variation(s_bb) 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.

• 핵의학기술
• /
• 제18권1호
• /
• pp.158-162
• /
• 2014

공인된 기구에 의해 발급된 문서를 동반하는 인증표준물질은 특성값과 추정값의 신뢰정도를 나타내는 연계 불확도, 그리고 측정한 결과가 명시된 불확정 정도의 범위 내에서 국가 측정 또는 국제측정표준에 일치되도록 연속적으로 비교하고 교정하는 소급성을 제공하는 표준물질이다. 회수율 검사는 검체를 측정하여 얻은 값이 참값에서 얼마만큼 벗어났는지의 차이를 말하며 키트의 정확도를 반영한다. 이러한 인증표준물질을 가지고 회수율 검사를 하는 것은 체외 방사면역진단키트의 정확성을 보여주며 이러한 평가는 매우 중요하다. 인증표준물질은 NIBSC (National Institute for biological standard and control, United Kingdom)와 IRMM (Institute for Reference Materials and Measurements, Belgium)에서 구입하였고 검사 종목은 T4, Ferritin, PSA, Prolactin, AFP 그리고 TSH으로 총 6종목이다. T4는 IRMM의 표준물질을 사용하였고 나머지 종목은 NIBSC의 표준물질을 사용하였다. C-1 (저농도), C-2 (중농도), C-3 (고농도) 3 level로 제조하여 본원에서 사용하는 키트를 이용하여 4회 측정하였다. WHO 인증표준물질을 이용한 회수율 측정에서 T4 90%, Ferritin 88%, PSA 94%, Prolactin 99%, AFP 94%, TSH 93%였다. 6개 종목의 회수율 측정에서 88-99%로 양호한 결과를 보였다. 핵의학 체외진단키트의 정확성을 높이기 위해서 이 연구가 다른 검사실의 키트로 확장되어 검사가 되어야 하고 검사실간에도 교류가 필요하다. 인증표준물질을 이용한 체외진단키트의 회수율 평가가 앞으로도 지속되어야 하며 결과의 정확성은 환자의 만족의 증가로 이어질 것으로 기대한다.

• Mass Spectrometry Letters
• /
• 제9권4호
• /
• pp.105-109
• /
• 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.

• Mass Spectrometry Letters
• /
• 제10권4호
• /
• pp.112-116
• /
• 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 (s_bb) and within-unit (s_wb) standard deviations are less than 2.5%, and the stability is found to be guaranteed for 50 days.

• 한국작물학회지
• /
• 제51권spc1호
• /
• pp.304-309
• /
• 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.

• 한국도서관정보학회지
• /
• 제36권2호
• /
• pp.283-305
• /
• 2005

과학기술데이터는 엄격한 평가기준에 의해 신뢰성과 정확성이 보장된 참조표준(standard reference data) 값을 지닐 수 있어야 한다. 참조표준은 측정표준을 바탕으로 구하여진 결과 값을 표준화시키는 작업으로서 데이터의 생산조건, 실험환경. 측정방법, 데이터 처리 등이 검토되어 참조데이터(reference data)와 구분된다. 참조표준은 "공인된 수치데이터"로 표현되고 이는 측정결과의 신뢰도를 정량적으로 나타내는 불확도 (uncertainty)로 표기된다. 본 연구에서는 참조표준에 대한 의미를 이해하고, 평가되지 않은 과학기술 데이터가 어떤 평가 과정을 거쳐 참조표준으로 분류되는지를 알아보기 위해 소재물성분야를 예로 살펴보았다. 그리고 국가 참조표준을 본격적으로 운영하기 위한 방안으로 국가참조표준센터, 데이터센터, 위원회의 역할과 임무, 이를 뒷받침하기 위한 법적. 제도적 방안을 제시하였다.

• 환경분석과 독성보건
• /
• 제21권4호
• /
• pp.209-219
• /
• 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.

• 한국진공학회지
• /
• 제11권4호
• /
• pp.218-224
• /
• 2002

반도체 박막의 분석에서 중요한 분석 대상의 하나인 미량 불순물의 정량분석을 위한 표준절차를 확립하고 그에 필요한 인증표준물질의 개발하였으며 이를 이용하여 국내공동분석을 실시하였다. 공동분석에 사용된 붕소가 균질하게 도핑된 박막 인증표준물질과 분석시편은 이온빔 스퍼터증착법에 의해 제작하였으며, 가장 정량적이고 감도가 높은 ICP-MS를 이용한 동위원소희석법으로 인증하였다. 이러한 인증표준물질과 SIMS에 의한 실리콘 내 의 붕소의 정량분석에 대해 이미 확립되어 있는 국제표준절차인 ISO/DIS-14237에 의거하여 국내 공동 분석을 시행하였는데, 이번의 공동분석에서 얻어진 붕소농도의 전체 평균값이 ICP-MS에 의한 인증치에 약 2% 정도의 오차를 보여주고 있어 분석의 정확성이 확인되었다.