Preparation of Al-doped mesoporous crystalline material-41 as fiber coating material for headspace solid-phase microextraction of polycyclic aromatic hydrocarbons from human urine
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 (R 2 ) 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%.
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