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학술연구/단체지원/교육 등 연구자 활동을 지속하도록 DBpia가 지원하고 있어요.
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Polychlorinated biphenyls (PCBs)은 산과 알칼리, 열에 안정하고 지용성의 특성을 갖는 잔류성 유기오염물질이다. 인체로의 유입 경로는 주로 음식물 섭취로 알려져 있으며, 국제암연구소(IARC)에서는 인체 발암성 물질인 그룹1로 규정하였다. 일반적으로, 식품 중 PCBs의 분석은 soxhlet extractor를 이용한 추출 과정, multi-layer silica column을 이용한 정제 과정 그리고 HRGC- HRMS에 의한 고감도 분석기기가 요구된다. 이에 본 연구에서는 헤드스페이스 고체상 미량 추출법(Headspace-solid phase micro extraction, HS-SPME)을 도입하여 분석시간 및 비용은 절감하고, GC-MS를 이용한 분석법을 연구하였다.
식품 시료는 지방의 함유와 물질의 유동성에 따라 4가지 매트릭스로 분류하였다. 비지방 액상은 20% 에탄올, 비지방 고체는 흰죽, 지방함유 액상은 우유, 지방함유 고체는 삼겹살로 대표매질을 선정하였다. 20% 에탄올과 흰죽은 HS-SPME 방법만을 적용하여 분석법을 확립하였다. 고지방 식품인 우유와 삼겹살은 LLE 방법으로 1차 추출 후 HS-SPME 방법을 적용하였다. 전처리 과정 후에는 GC-MS를 이용하여 indicator PCBs 7종을 동시에 정량 및 정성분석 하였다. 그 결과 직선성, 정밀도, 정확도 등이 양호하였으며, 비용적인 측면과 분석시간 등을 모두 고려하였을 때 매우 효율적임을 확인하였다. 20% 에탄올과 흰죽을 분석한 결과 검출한계가 0.2-10 pg/g 수준이었고, 지방함유 시료인 우유와 삼겹살은 10-5000 pg/g 수준까지 분석이 가능하였다. 이에 본 연구에서 제시한 HS-SPME를 이용한 분석법은 지방 함유 식품 중 저분자량을 가지는 휘발성 PCBs를 대상으로 모니터링에 적용할 수 있을 것으로 사료된다.
식품 시료는 지방의 함유와 물질의 유동성에 따라 4가지 매트릭스로 분류하였다. 비지방 액상은 20% 에탄올, 비지방 고체는 흰죽, 지방함유 액상은 우유, 지방함유 고체는 삼겹살로 대표매질을 선정하였다. 20% 에탄올과 흰죽은 HS-SPME 방법만을 적용하여 분석법을 확립하였다. 고지방 식품인 우유와 삼겹살은 LLE 방법으로 1차 추출 후 HS-SPME 방법을 적용하였다. 전처리 과정 후에는 GC-MS를 이용하여 indicator PCBs 7종을 동시에 정량 및 정성분석 하였다. 그 결과 직선성, 정밀도, 정확도 등이 양호하였으며, 비용적인 측면과 분석시간 등을 모두 고려하였을 때 매우 효율적임을 확인하였다. 20% 에탄올과 흰죽을 분석한 결과 검출한계가 0.2-10 pg/g 수준이었고, 지방함유 시료인 우유와 삼겹살은 10-5000 pg/g 수준까지 분석이 가능하였다. 이에 본 연구에서 제시한 HS-SPME를 이용한 분석법은 지방 함유 식품 중 저분자량을 가지는 휘발성 PCBs를 대상으로 모니터링에 적용할 수 있을 것으로 사료된다.
목차
1. 서론 ··················································································································· 12. 실험방법 ············································································································· 52.1 시약과 표준용액 ························································································· 52.2 시료의 분류(대표매질 선정) ···································································· 92.3 시료 전처리 방법 ····················································································· 112.3.1 비지방 액체(20% 에탄올) 전처리 방법 ·········································· 112.3.2 비지방 고체(흰죽) 전처리 방법 ······················································· 122.3.3 지방 액체(우유) 전처리 방법 ··························································· 132.3.4 지방 고체(삼겹살) 전처리 방법 ······················································· 152.4 정도 관리 ··································································································· 172.4.1 검정곡선 작성 및 검출한계 ···························································· 172.4.2 정밀도와 정확도 ················································································ 172.5 기기 분석 ··································································································· 183. 결과 및 고찰 ··································································································· 213.1 분석 조건의 최적화 ················································································· 213.2 정도 관리 ··································································································· 343.2.1 검정곡선 작성 및 검출한계 ···························································· 343.2.2 정밀도와 정확도 ················································································ 373.3 선행연구와의 분석 결과 비교 ······························································· 424. 결론 ··················································································································· 445. 참고문헌 ········································································································· 466. ABSTRACT (in English) ················································································ 51
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