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Determination of 16 Polycyclic Aromatic Hydrocarbons in Roast Duck Skin by Gel Permeation Chromatography Clean-up Combined with Gas Chromatography-Mass Spectrometry |
SHEN Xixi, ZHAN Junliang, TANG Xiaoyan |
1.Key Laboratory of Meat Processing and Quality Control, Ministry of Education, College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China; 2.Key Laboratory of Agri-Food Safety and Quality, Ministry of Agriculture, Institute of Quality Standards and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China |
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Abstract This study established an analytical method for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in Beijing roast duck skin by gel permeation chromatography (GPC) clean-up combined with gas chromatography-mass spectrometry (GC-MS). After homogenization, samples were extracted ultrasonically with ethyl acetate, and the extract was purified by GPC before being analyzed. The results showed that the calibration curves for the 16 PAHs were all linear in the concentration range of 1–100 μg/L with correlation coefficients (R2) above 0.996, the limits of detection (LOD) ranged from 0.08 to 0.39 μg/kg, and the limits of quantification (LOQ) ranged from 0.25 to 1.29 μg/kg. At spiked levels of 1, 5, and 10 μg/L, the recoveries of the method ranged from 66.2% to 108.3%, with relative standard deviations (RSD) of 0.7% to 13.5% (n = 6), which met the requirements for quantitative analysis. When this method was applied to Beijing roast ducks purchased from supermarkets, no benzo(a)pyrene was detected in duck skin samples, and the total content of PAH4 (benz(a) anthracene, chrysene, benzo(b)fluoranthene, benzo(a)pyrene did not exceed the EU limit (12.0 μg/kg).
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