The Al-doped mesoporous crystalline material-41 (Al-MCM-41) composite was prepared and applied as fiber coating material of headspace solid-phase microextraction (HS-SPME) for extraction of polycyclic aromatic hydrocarbons (PAHs) from human urine. Five PAHs including acenaphthene, fluorene, phenanthrene, anthracene, and pyrene are chosen as target analytes to evaluate the performance of the material by GC-FID analysis. The mesoporous Al-MCM-41 composite was characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, nitrogen adsorption/desorption measurement, and thermogravimetric analysis. The parameters affecting the extraction efficiency of HS-SPME were investigated. Under the optimal conditions, the method exhibits ideal linearity for target analytes in the range of 0.3–600 ng⋅mL^-1 with the coefficients (R²) equal or higher than 0.9906. The enrichment factors are calculated from 540 to 1760. The limits of detection (LODs) and limits of quantitation (LOQs) are between the ranges of 0.06–0.18 and 0.3–0.9 ng⋅mL^-1, respectively. The relative standard deviations (RSDs) (n = 5) of intra-day and inter-day are in the ranges of 1.08–7.49% and 2.84–18.3% respectively. The fiber-to-fiber reproducibility (n = 3) is in the range of 6.47–13.9%. The method was successfully applied for the analysis of PAHs in human urine with reasonable recoveries which is ranging from 73.29 to 116.1%.

制备了Al掺杂的介孔晶体材料41（Al-MCM-41）复合材料，并将其用作顶空固相微萃取（HS-SPME）的纤维涂料，用于从人尿液中提取多环芳烃（PAHs）。选择了五种PAH，包括including，芴，菲，蒽和pyr作为目标分析物，以通过GC-FID分析评估材料的性能。通过扫描电子显微镜，透射电子显微镜，X射线衍射，傅立叶变换红外光谱，氮吸附/解吸测量和热重分析来表征介孔Al-MCM-41复合材料。研究了影响HS-SPME萃取效率的参数。在最佳条件下^-1，系数（R ²）等于或大于0.9906。富集因子的计算范围为540至1760。检测限（LODs）和定量限（LOQs）分别在0.06-0.18和0.3-0.9 ng·mL ^-1之间。 日内和日间相对标准偏差（RSD）（n = 5）分别在1.08–7.49％和2.84–18.3％的范围内。光纤到光纤的可重复性（n  = 3）在6.47-13.9％的范围内。该方法成功用于人尿中多环芳烃的分析，回收率合理，在73.29％至116.1％之间。