气相色谱/质谱法测定烧烤肉制品中15种欧盟优控多环芳烃

Analysis of 15 European Priority Polycyclic Aromatic Hydrocarbons in Grilled Meat Samples Using Gas Chromatography Coupled with Mass Spectrometry

建立了一种快速、灵敏的测定烧烤肉制品中15种欧盟优控多环芳烃(PAHs)方法。以环己烷为溶剂,对5g均质样品进行加压液体萃取,并在萃取池中加入佛罗里硅土对脂肪进行预处理。萃取液经凝胶净化除去大分子脂肪酸,再经硅胶固相萃取柱进一步净化,以4mL环己烷洗脱。洗脱液最终浓缩定容至1mL,采用气相色谱/质谱法对目标化合物进行定性和定量检测。本研究利用全因子实验设计和中心复合实验设计方法对3个色谱进样参数(进样口温度、脉冲时间和不分流时间)的取值进行优化。本方法检出限为0.20～0.91μg/kg。对所有目标化合物,方法线性关系均良好(r>0.99)。日内精密度和日间精密度均小于10%。在两个加标水平下,15种PAHs平均回收率为72.6%～96.9%。使用本方法对市售的5个烧烤肉制品进行检测,样品中PAHs浓度为0.87～19.52μg/kg。

An efficient and selective analytical method for the determination and the quantification of 15 European priority polycyclic automatic hydrocarbons 15 EU priority PAHs in grilled meat samples has been devel-oped.Approximately 5 g of homogenised sample was extracted using pressurized liquid extraction （PLE） with a stationary phase of florisil added in the cell to assure a preliminary purification of the extract.Then the gel permeation chromatography （GPC） was used to remove the lipids in the evaporated PLE-extract followed by purification with 5 g preconditioned silica SPE cartridge.Afterwards,the PAH fraction was eluted with 4 mL of cyclohexane and concentrated for GC-MS analysis.In addition,three injection parameters of the GC-MS analysis （injection temperature,pulse injection time and splitless injection time） were optimized by applying experimental designs.Limits of detection varied from 0.20 to 0.91 μg/kg for PAHs in grilled meat were obtained.The calibration curves showed a good linearity for all PAHs （R20.99） .The precision （RSD10% ） and recovery （between 72.6% and 96.9% ） were fit for purpose.The method was then applied to the determination of PAHs in five grilled meat samples obtained from a local market.15 EU priority PAHs were found to be present at levels ranging from 0.87 to 19.52 μg/kg wet sample.