GC-tandem mass spectrometry를 이용한 분쇄원두커피 및 식용유지중 polycyclic aromatic hydrocarbons 분석법 연구

Abstract

Polycyclic aromatic hydrocarbons (PAHs) are well-known chemical compounds, which are found in the environment as pollutants and have been identified as human carcinogens. The purpose of this study is to develop a rapid analytical method for determining 15 PAHs of EU priority in ground coffee, sesame oil, and perilla oil using GC-tandem mass spectrometry. The linearity of standard mixture of PAHs in the range of 0.5 ~ 20 ㎍/㎏ was satisfactory with correlation coefficients (R2) of 0.9941 ~ 0.9999 except for dibenzo(a,h)pyrene. In order to evaluate the sample preparation methods, PAHs of ground coffees were analyzed after being extracted using the methods such as saponification -liquid-liquid extraction, soxhlet extraction, and solid-liquid extraction. Among the tested extraction methods, solid-liquid extraction method showed best repeatability and efficient reduction of matrix effect. LODs of solid -liquid extraction method for ground coffees were 0.002~0.1 ㎍/㎏ and LOQs were 0.006~0.2 ㎍/㎏. PAHs in edible oils were analyzed using direct SPE method. LODs of direct SPE method in edible oils were 0.05~2.5 ㎍/㎏ and LOQs were 0.15~5.0 ㎍/㎏. The recovery values for ground coffee and oil ranged 52.6~93.3 % and 55.1~ 105.0% respectively. Validation of this method was measured with the CRM (Institute for Reference Materials and Measurements BCR 458), and the error values ranged 2.06 ~ 4.30% as a result. 46 commercial ground coffee and 14 sesame oils, and 7 perilla oils were analyzed to determine their PAHs contamination levels. The PAHs concentration in ground coffees and edible oils ranged N.D ~ 5.988 ㎍/㎏ and N.D ~ 29.627 ㎍/㎏ respectively. Only one sample had excess benzo(a)pyrene, which was more than 2.0 ㎍/㎏. GC-tandem mass spectrometry for 15 PAHs quantitation showed better resolution and lower LODs than GC-MS-SIM and HPLC-FLD. The proposed preparation method can be applied to the analysis of PAHs in ground coffees and edible oils. This study was conducted with TEFs(Toxic Equivalency Factors), U.S.EPA recommendation to identify dietary risk for PAHs in coffees, sesame oils, and perilla oils. The estimated average daily dose of PAHs was 5.24 × 10-8 mg/kg b.w./day for coffees, 5.02 × 10-9 mg/kg b.w./day for sesame oils, and 1.11 × 10-9 mg/kg b.w./day for perilla oils.