보고서 정보
주관연구기관 |
KOTITI시험연구원 KOTITI Testing & Institute |
보고서유형 | 최종보고서 |
발행국가 | 대한민국 |
언어 |
한국어
|
발행년월 | 2015-11 |
과제시작연도 |
2015 |
주관부처 |
식품의약품안전청 Korea Food & Drug Administration |
등록번호 |
TRKO201600010309 |
과제고유번호 |
1475008432 |
사업명 |
식품 등 안전관리 |
DB 구축일자 |
2016-10-15
|
키워드 |
식품첨가물.동클로로필.동.직접 분석법.food additives.copper chlorophyll.copper.direct method.
|
DOI |
https://doi.org/10.23000/TRKO201600010309 |
초록
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본 연구는 국내외 문헌조사, 시료 전처리 및 기기분석 조건 검토를 통한 식품 중 동클로로필 간접추정법(동(Cu)로서) 및 직접 분석법을 확립하고자 수행되었다. 또한, 국내유통 식품 중동(Cu) 및 동클로로필 함유량 분석을 통해 확립된 분석법의 적용성을 검토하였다.
식품 중 동클로로필 간접 추정방법을 확립하기위하여 일반식품 군은 microwave를 이용하여 분해하였으며, 해조류 및 고분자 화합물을 함유한 식품(다시마, 추잉껌, 한천, 유지류)의 경우 균질화된 시료(0.1~0.5g)를 microwave vessel에 취한
본 연구는 국내외 문헌조사, 시료 전처리 및 기기분석 조건 검토를 통한 식품 중 동클로로필 간접추정법(동(Cu)로서) 및 직접 분석법을 확립하고자 수행되었다. 또한, 국내유통 식품 중동(Cu) 및 동클로로필 함유량 분석을 통해 확립된 분석법의 적용성을 검토하였다.
식품 중 동클로로필 간접 추정방법을 확립하기위하여 일반식품 군은 microwave를 이용하여 분해하였으며, 해조류 및 고분자 화합물을 함유한 식품(다시마, 추잉껌, 한천, 유지류)의 경우 균질화된 시료(0.1~0.5g)를 microwave vessel에 취한 후 120℃로 가열하여 예비분해를 거친 후 microwave를 이용하여 분해하였다. 분해액을 시험용액으로 사용하여 ICP-OES로 동(Cu) 함량을 분석하였다. 분석법 검증 결과, 회수율은 약 93.3~96.2%, 정밀성(%RSD)은 2.7~4.5% 이하, 검출 및 정량한계는 각각 0.43 μg/kg, 1.43 μg/kg, 직선성(R2)은 0.999이었다.
동클로로필 직접 분석법은 유지류의 경우 시료를 석유에테르 5ml에 녹인 후 실리카 카트리지에 주입하여 석유에테르와 에테르 혼합용매로 수세하여 비극성 물질을 제거한 후 아세톤 용매로 용리한 다음 이를 질소가스 하에서 농축하여 시험용액으로 사용하였다. 유지류 이외의 식품군에서는 아세톤으로 동클로로필을 추출한 후 질소가스 하에서 아세톤을 제거하고 에테르로 재용해하여 실리카 카트리지에 주입 후 유지류와 같은 방법으로 분석하였다. 분석법 검증 결과, 회수율은 약 90.4~108.2%, 정밀성(%RSD)은 3.2~4.7% 이하, 검출 및 정량한계는 각각 0.01 mg/kg, 0.04 mg/kg, 직선성(R2)은 0.999로 우수하였다. 또한, 측정불확도도 산출하였다.
확립된 분석법을 국내유통 식품에 적용을 통한 검증을 위해 일부 식품 중 동(Cu) 및 동클로로필 함량을 분석하였다. 시중 유통 중인 7개 식품군(다시마, 과실류저장품, 채소류 저장품, (365건)을 구입하여 분석하였다. 간접 추정법 적용시 동(Cu) 함량은 미량 검출되었으나 문헌 등을 통해 천연유래로 판단되었으며, 동클로로필은 모든 시료에서 불검출이었다.
본 연구에서 확립된 분석법은 식품 중 동클로로필 안전관리 강화를 위해 기초자료로 활용될 것으로 기대된다.
Abstract
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The purpose of this research was to develop quantitative analytical method for copper chlorophyll pigment in foods by HPLC. We have examined the applicability of new developed method for copper chlorophyll by applying to processed foods and investigated the content of copper (Cu) and copper chloroph
The purpose of this research was to develop quantitative analytical method for copper chlorophyll pigment in foods by HPLC. We have examined the applicability of new developed method for copper chlorophyll by applying to processed foods and investigated the content of copper (Cu) and copper chlorophyll in permitted foods which are sold in markets.
In order to establish the indirect estimation method for chlorophyll, the foods that belong to common food groups have decomposed utilizing the microwave. Seaweed and foods containing high molecular compounds such as kelp, chewing gum, agar, fats and oils were found to require a pre-decomposed step by heating at 120 ℃ because the violent reaction could occur during the decomposition. After the pre-treatment step, the foods decomposed with microwave and the decomposed solution was analyzed as the amount of Cu by ICP-OES.
The validation of analytical method was carried out by determining recovery experiment, sensitivity, LOD, LOQ and precision. Theresults indicated that the recovery values (%) of Cu were 93.3 to 96.2 by indirect measurement method through the analysis,and relative standard deviation (RSD, %) range was 2.7 to 4.5 or less, limits of detection (LOD) and limits of quantification (LOQ) values were 0.43 μg/kg and 1.43 μg/kg, respectively. The correlation coefficient (R2) value was 0.999.
In the case of fatty foods, the sample was dissolved in 5 mL petroleum ether and then transferred to silica cartridge. Non-polar materials in foods were removed by the addition of solvent system of petroleum ether and ether,and copper chlorophyll was eluted by acetone. The eluted solution was analyzed after concentrating it under the nitrogen gas.
With the exception of the fatty foods group, Copper chlorophyll was extracted using acetone and then removed by nitrogen gas. The extracted copper chlorophyll was resolved by ether and transferred to silica cartridge. The followed step was same with that of used in fatty foods analysis.
The validation analytical method including recovery experiment, sensitivity, LOD, LOQ, method precision was carried out. The results indicated that the recovery values(%) of Cu was 90.4 to 108.2 by indirect measurement method through the analysis and relative standard deviation (RSD, %) was 3.2 to 4.7 or less, limits of detection (LOD) and limits of quantification, 0.01 mg/kg and 0.04 mg/kg respectively. linearity (R2) is 0.999. Also, we have to calculate the uncertainty of measurement of each analytical method.
The established analytical method for verification through the application of domestic distribution food, we analyzed some of the same chlorophyll content with the food in the copper (Cu). Commercial distribution ofseven food groups (kelp, fruits stored products, such as vegetables supplies. etc) was analyzed to buy 365 samples.
When direct estimation method was applied, the content of the Cu which was detected in traces as reported in few literatures is determined to be natural; the chlorophyll was not detected in all samples.
It is concluded that the new established analytical method could be used for the enforcement of the safety management of copper chlorophyll.
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