식품 중 다이옥신(2,3,7,8-Tetrachlorodibenzo-p-dioxin) 분석 시 측정불확도 추정

• Published in: Han'guk Sikp'um Yŏngyang Kwahakhoe chi Vol. 50; no. 8; pp. 832 - 842
• Main Authors: 박찬종(Chan Jong Park), 김한솔(Han Sol Kim), 안태현(Taehyun Ahn), 정은아(Eun A Chong), 이지은(Ji Eun Lee), 서수진(Sujin Seo), 구용의(Yong Eui Koo)
• Format: Journal Article
• Language: Korean
• Published: 한국식품영양과학회 01.08.2021
• Subjects: 식품과학; measurement uncertainty; standardization; dioxin; ISO/IEC 17025; quality assurance
• ISSN: 1226-3311; 2288-5978

본 연구에서는 식품 중 다이옥신 분야 ISO/IEC 17025 인정 획득을 통한 국제기준에 부합하는 품질보증체계를 마련하기 위하여 식품 중 다이옥신(2,3,7,8-TCDD)을 분석하는 과정에서 중요한 불확도 요인들(실험실 내 정밀도, 정확도, 검량선, 시료의 반복 측정, 표준물질, 내부표준물질의 농도, 시험용액의 부피, 시료의 무게 측정) 8가지를 선정하고 그 측정 결과에 대한 불확도를 추정하였다. 불확도 측정에 대한지침서(GUM) 및 Eurachem 가이드라인에 근거하여 불확 추정 모델 관계식을 설정하였다. 요인 각각에 대한 불확도를 구한 후 2,3,7,8-TCDD 농도에 대한 합성표준불확도를 산출한 결과, 1.9 pg/g으로 나타났으며 확장불확도는 3.8 pg/g으로 산출되었다. 불확도를 고려하여 표현된 최종 2,3,7,8-TCDD 농도는 12.0±3.8 pg/g이다. 또한 불확도 요인별 기여율은 시험의 정확도(41%)가 가장 크게 나타났고, 실험실 내 정밀도(22%), 표준물질(13%), 시료의 반복 측정(12%), 시험용액의 부피(6%), 검량선(3%), 내부표준물질(3%)의 순서로 나타났고, 시료의 무게 측정(0%)은 영향을 주지 않았다. In this study, the quality assurance system was established in line with international standards by acquiring ISO/IEC 17025 accreditation for dioxin analysis in food. In order to strengthen the reliability and public credibility of the results, ISO/IEC 17025 recommends to provide information on ‘measurement uncertainty’ along with the measured values. Based on the ‘Guide to the Estimation of Uncertainty in Measurement’ (GUM) and the ‘EURACHEM/CITAC guide’, a model relational equation for estimating the uncertainty of the 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8- TCDD) analysis in food was established. In the process of analyzing the 2,3,7,8-TCDD concentration in food, the measurement uncertainty was calculated by considering the important uncertainty factors that may exist. The combined uncertainty was calculated by using the eight uncertainty factors (precision, recovery, calibration curve, repeat measurement of sample, standard, internal standard, volume of sample, and weight of sample). The biggest factor influencing the uncertainty was the recovery. In the 95% confidence interval, the expanded uncertainty was calculated as 3.8 pg/g using k-value (2). The final expression can be stated as 12.0±3.8 pg/g (confidence interval 95%, k=2). Through the measurement uncertainty estimation, the factors that cause analysis errors during the analytical procedure of dioxin were identified and the degree of their influence on the results was calculated. The reliability of the analysis result was obtained by calculating the uncertainty, which is the basic element of ISO/IEC 17025 and minimizing the uncertainty factors. KCI Citation Count: 0