该研究建立了高效液相色谱（High Performance Liquid Chromatography，HPLC）同时分析香辛料中15种多环芳烃类污染物（Polycyclic Aromatic Hydrocarbons，PAHs）含量的内标检测方法。样品经氢氧化钠溶解，乙腈萃取，正己烷复溶后，过弗罗里硅土（Florisil）小柱净化浓缩，供HPLC检测，苯并[a]芘-D12作为内标定量。该方法在0~100 ng/mL内线性关系良好，辣椒中PAHs检出限：0.5~3.0 μg/kg；定量限2.0~10.0 μg/kg；花椒中检出限：0.5~1.0 μg/kg；定量限2.0~3.0 μg/kg。在2.0、10.0、50.0 μg/kg 3个浓度水平，辣椒中回收率范围为60.58%~119.48%，相对标准偏差（Relative Standard Deviations，RSD）（n=6）为1.25%~9.61%，花椒中回收率为60.46%~119.24%，RSD（n=6）为1.10%~8.56%。5种地产香辛料中ΣPAHs 含量由高到低为：青花椒（561.2 μg/kg）＞二荆条（448.8 μg/kg）＞红花椒（358.3 μg/kg）＞石柱红（353.6 μg/kg）＞小米辣（243.5 μg/kg），区县种植基地污染较严重的为璧山、江津和荣昌，ΣPAHs分别为721.5、626.6和621.0 μg/kg，PAHs中污染较严重的化合物为菲、荧蒽和芘，平均含量分别为215.10、80.25和75.35 μg/kg。该研究建立的内标法准确度高，重复性好，适用于香辛料及制品中PAHs检测。

An internal standard HPLC method was established for simultaneous determination of 15 kinds of PAHs in spices by. The samples were dissolved in sodium hydroxide, extracted with acetonitrile, redissolved by n-hexane, cleaned and concentrated by the Florisil SPE cartridge, and determined by HPLC, with benzo [a] pyrene D12 being used as the internal standard. This method had a good linear relationship in the range of 0~100 ng/mL, with the detection limits of PAHs in Capsicum being 0.5~3.0 μg/kg and the limits of quantitation as 2.0~10.0 μg/kg. The limits of detection and limits of quantitation of PAHs in Zanthoxylum were 0.5~1.0 μg/kg and 2.0~3.0 μg/kg, respectively. When the spiked levels were 2.0, 10.0 and 50.0 μg/kg, the recoveries in the two spices were 60.58%~119.48% and 60.46%~119.24%, with the RSD (n=6) being 1.25%~9.61% and 1.10%~8.56%. The concentration of ΣPAHs in the five spices from high to low were : green Zanthoxylum (561.2 ųg/kg) > erjingtiao (448.8 μg/kg) > red Zanthoxylum (358.3 μg/kg) > shizhuhongi (353.6 μg/kg) > chilli (243.5 μg/kg). The more seriously polluted areas of Chongqing were Bishan, Jiangjin and Rongchang, with ΣPAHs being 721.5, 626.6 and 621.0 μg/kg, respectively. The more seriously polluted compounds in PAHs were phenanthrene, fluoranthrene and pyrene, with their average contents being 215.10, 80.25 and 75.35 μg/kg, respectively. The internal standard method established in this study has high accuracy and good repeatability, which is suitable for the determination of PAHs in spices.

重庆市市场监督管理局科研计划项目（CQSJKJ2022006）