고체상추출법과 GC/MS-SIM을 이용하여 볶음 처리한 곡류 중 아크릴아마이드 분석 (Determination of Acrylamide using Solid-phase Extraction and Gas Chromatography-Mass Spectrometry Selected Ion Monitoring in Roasted Cereal Foods)

서지정보

· 발행기관 : 대한환경공학회
· 수록지 정보 : 대한환경공학회지 / 41권 / 4호 / 214 ~ 220페이지
· 저자명 : 유대영, 이장미, 김혜경, 장철현

초록

본 연구는 토양 또는 수계에 유입되어 오염을 일으킬 가능성이 있는 볶음 처리한 곡류 차 중 아크릴아마이드 분석방법을 검토하였다. 제시된 방법은 아크릴아마이드를 증류수로 추출한 후 고체상 추출법(solid phase extraction, SPE)을 이용하여 간섭 요인을 제거하고 브롬화 유도체화 반응을 최적화하여 생성된 2,3-dibromopropionamide를 ethyl acetate로 추출하여GC/MS (SIM)분석하였다. 고체상 추출법(SPE)은 활성탄이 충진된 Supelclean TM Coconut Charcoal cartridge를 사용하였다. 그결과 분석방법의 방법검출한계(MDL)는 0.76 μg/kg이고, 정량한계(LOQ)는 2.32 μg/kg이였다. 검정곡선의 직선성 상관계수(R 2 )는 2.5~100 μg/kg의 농도범위에서 0.9997을 나타내었다. 그리고 정밀도(precision)와 정확도(accuracy)는 5.3~5.6% 이내로안정적이었으며, 회수율(recovery)은 95.8~104%로 측정되었다.

영어초록

An analytical method has been developed for the determination of acrylamide in cereal-based foods. The method is based on extraction of acrylamide with water, cleaned up through a solid phase extraction (SPE) cartridge, followed by bromination of the acrylamide double bond. The reaction product (2,3-dibromopropionamide) is extracted with ethyl acetate and analyzed by gas chromatography coupled to mass spectrometry (GC/MS) in selected ion monitoring (SIM), employing acrylamide- 2,3,3-d3 (AA-d3) as internal standard. The SPE process for sample preconcentration was performed on a commercially available Supelclean TM Coconut Charcoal cartridge packed with active carbon. In this method, correlation coefficients (R 2 ) of calibration curves appeared to be 0.9997 in the concentration range of 2.5~100 μg/kg. The method detection limit (MDL) and the limit of quantitation (LOQ) of acrylamide were 0.76 μg/kg and 2.32 μg/kg, respectively. The calibration curve showed good linearity above 0.9997 in the ranges of the 2.5~100 μg/kg. For validation purposes, recovery studies were carried out at one concentration levels (10 μg/kg, n=3). The intraday assay accuracy and precision were in the range 104% and 5.6%, respectively, and the interday assay accuracy and precision were in the range 95.8% and 5.3%, respectively.

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