凝胶渗透色谱净化-气相色谱-质谱法检测烤鸭鸭皮中16种多环芳烃

Determination of 16 Polycyclic Aromatic Hydrocarbons in Roast Duck Skin by Gel Permeation Chromatography Clean-up Combined with Gas Chromatography-Mass Spectrometry

建立北京烤鸭鸭皮中16种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)的凝胶渗透色谱(gel permeation chromatography,GPC)净化-气相色谱-质谱(gas chromatography-masss pectrometry,GC-MS)检测分析方法。匀浆后的烤鸭鸭皮样品经乙酸乙酯超声提取20 min,采用GPC净化,GC-MS进行检测。结果表明:16种PAHs在1~100μg/L质量浓度范围内线性关系良好(R^2>0.996),检出限为0.08~0.39μg/kg,定量限为0.25~1.29μg/kg;在1、5、10μg/kg添加水平下,16种PAHs的回收率为66.2%~108.3%,相对标准偏差为0.7%~13.5%(n=6),满足分析要求;采用该方法对购自超市的北京烤鸭进行检测,烤鸭鸭皮样品中均未检出苯并(a)芘,苯并(a)芘、苯并(a)蒽、苯并(b)荧蒽和?总含量也未超过欧盟限量标准(12.0μg/kg)。

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(R^2) 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).