分子印迹固相萃取-同位素内标-GC-MS/MS法测定种子果实类中药材中18种多环芳烃残留量及其初步风险评估

Determination and Preliminary Risk Assessment of 18 Polycyclic Aromatic Hydrocarbons in Seed-Fruit Herbs by Molecular Imprinting Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry

目的建立了分子印迹固相萃取-同位素内标-气相色谱质谱联用(GC-MS/MS)法测定种子果实类中药材中18种多环芳烃的残留量的方法,并对其进行初步风险评估,为评价种子果实类中药材安全性提供有效分析手段。方法采用氘代多环芳烃同位素内标,样品以正己烷提取,经分子印迹固相萃取小柱净化后,采用GC-MS/MS法测定,色谱柱为DM-17ms(0.25 mm×30 m,0.25μm),程序升温,以多反应离子监测模式进行检测。采用毒性当量因子法对种子果实类中药材中多环芳烃进行初步风险评估。结果18种多环芳烃在2~50 ng·mL^(-1)内线性关系良好;在2~50μg·kg^(-1)内的平均回收率为77.25%~112.32%,相对标准偏差(RSD)为2.74%~15.89%(n=3);方法定量限为0.2~1μg·kg^(-1)。根据风险评估结果,部分品种ILCR值介于10-4与10-6之间。结论本方法操作简便、专属性强、灵敏度高,可满足种子果实类中药材中18种多环芳烃残留的定量检测工作。部分种子果实类中药多环芳烃残留量可能存在潜在致癌风险,需要引起注意。

OBJECTIVE To research and evaluate risk of 18 polycyclic aromatic hydrocarbons(PAHs)in seed-fruit herbs based on a SPE-isotope dilution GC-MS/MS method for the determination of the residues.METHODS Using isotope as internal standard,the sample was extracted by n-hexane and purified by molecular imprinting solid phase extraction.GC-MS/MS method was used for the assay.The chromatographic column was DB-17ms(0.25 mm×30 m,0.25μm)with temperature programming and MRM detection.The preliminary risk assessment of polycyclic aromatic hydrocarbons(PAHs)in seeds and fruits of traditional Chinese medicine(TCM)was carried out by using toxicity equivalent factor method.RESULTS The calibration curves for the 18 kinds of typical PAHs were linear in the range of 2-50 ng·mL^(-1).The average recovery rate was in the range of 77.25%-112.32%,with RSD 2.74%-15.89%(n=3).The LOQs were 0.2-1μg·kg^(-1)According to the risk assessment results,some varieties may have potential cancer risk.CONCLUSION This method is specific,sensitive,and can be used for residue detection of 18 typical kinds of PAHs in seed-fruit herbs.The residual amount of PAHs in some seeds and fruits of traditional Chinese medicine may have a potential cancer risk,which need attention.