밀에서 HPLC에 의한 데옥시니발레놀 분석의 측정불확도 산정

국문 초록 (Abstract)

본 연구에서는 밀 시료에서 면역친화컬럼을 이용한 HPLC분석법으로 데옥시니발레놀을 분석함에 있어서 발생될 수 있는 측정 불확도를 GUM 지침에 따라 산정하였다. 분석과정에서의 불확도 요인은 시료량 측정, 최종 시료부피, 보관표준용액, 작업표준용액, 표준용액, 기기, 매질, 검량선 작성으로 구분하였다. 불확도 요인의 구성요인은 저울의 안정성, 분해능, 재현성, 표준물질의 순도, 분자량, 농도, 표준용액 희석, 검량선, 회수율 및 분석기기의 재현성 등이 작용하였다. 공시료에 데옥시니발레놀 300 μg/kg을 첨가하여 분석한 결과 255.29±71.62 μg/kg으로 측정되었다. 확장불확도는 합성표준불확도 35.81 μg/kg에 포함인자(k=2, 신뢰수준 95%)를 곱하여 산출하였다. 밀에서 데옥시니발레놀을 분석함에 있어 불확도에 영향을 주는 주요인자는 시료의 회수율과 검량선 작성인 것으로 파악되었다. 따라서 밀 시료에서 데옥시니발레놀 분석의 정밀성을 높이기 위해서는 회수율과 검량선 작성에 영향을 끼칠 수 있는 면역친화컬럼에 의한 시료의 정제과정과 표준물질의 희석과정에 주의를 기울이고 주기적으로 마이크로피펫을 교정하는 등 세심한 관리가 필요할 것으로 판단된다.

다국어 초록 (Multilingual Abstract)

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 μg/kg was estimated as 71.62 μg/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.

목차 (Table of Contents)

• Abstract
• 서론
• 재료 및 방법
• 결과 및 고찰
• 요약
• 문헌

참고문헌 (Reference)

1 FAO, "Worldwide regulations for mycotoxins in food and feed in 2003" Food and Agriculture Organization 2004

2 Chun HS, "Safety evaluation of deoxynivalenol, a Fusarium mycotoxins, in food" Korea Food & Drug Administration 2007

3 Joint FAO/WHO Expert Committee on Food Additives, "Safety evaluation of certain mycotoxins in food. Prepared by the Fiftysixth meeting of JECFA. WHO food additives series 47/FAO food and nutrition 74"

4 EU, "Report on the relationship between analytical results, measurement uncertainty, recovery factors and the provisions of EU food and feed legislation, with particular reference to community legislation concerning"

5 USDA, "Quantitative test kit for deoxynivalenol for wheat, malted barley, barley, oats, corn. FGIS 2002-104"

6 EURACHEM, "Quantifying uncertainty in analytical measurement 2nd"

7 EURACHEM, "Quantifying uncertainty in analytical measurement"

8 AOAC, "Official Methods of Analysis of AOAC international. 18th ed. Method 986.18"

9 AOAC, "Official Methods of Analysis of AOAC international. 18th ed. Method 986.17"

10 Pei SC, "Occurrence of deoxynivalenol in Korean barley and barley products" 62 : 93-96, 2004

11 IARC, "Monographs on the evaluation of carcinogenic risks to humans: Some naturally occurring substances, food items and constituents, heterocyclic aromatic amines and mycotoxins" International Agency for Research on Cancer 1993

12 KOLAS, "Guideline for quantifying and expressing the uncertainty in measurement results"

13 ISO, "Guide to the expression of uncertainty in measurement"

14 KRISS, "Guide to the Expression of Uncertainty in Measurement"

15 FSA, "Food standards agency information bulletin on methods of analysis and sampling for foodstuffs. No. 59"

16 WHO, "Evaluation of certain mycotoxins in food. Fifty-sixth report of the Joint FAO/WHO expert committee on food additives" WHO 35-42, 2002

17 CODEX Committee on Contaminants in Foods, "Discussion paper on deoxynivalenol. Joint FAO/WHO food standards programme CODEX committee on contaminants in foods. First session" Food and Agriculture Organization 2007