Abstract:
0.05 g of sample was taken and placed in a 50 mL-centrifuge tube. 10 mL of
n-hexane was added, and the mixture was sonicated for 20 min and centrifuged for 10 min. The supernatant was taken and placed in another 50 mL-centrifuge tube. The extraction of the residue was repeated with
n-hexane once,and the supernatant was combined and blown to 2-3 mL by nitrogen at 40 ℃. The solution was purified with Macklin chromatography silica gel self-made chromatography column,and 70 mL of
n-hexane was added for rinsing. The eluent was blown to 2 mL by nitrogen at 40 ℃ and the solution was passed through an Agela Cleanert Bap-3 extraction column (activated with 5 mL of dichloromethane and 5 mL of
n-hexane). 10 mL of
n-hexane (5 mL each time) and 5 mL of dichloromethane were added in sequence for rinsing. The eluent was blown to near dryness by nitrogen at 40 ℃, and 1.0 mL of acetonitrile was added. The mixture was vortexed for 0.5 min and passed through a 0.22 μm organic filter membrane. The filtrate was analyzed by high performance liquid chromatograph. Waters PAH C
18 column was used as the stationary phase and the mixed solution composed of acetonitrile and water at different volume ratios was used as the mobile phase for gradient elution. As shown by the results, linear relationship between the corresponding peak areas and mass concentrations of benzoapyrene was found in the range of 5.00-500.0 μg·L
-1, with detection limits (3S/N) of 10 μg·kg
-1. RSDs (
n=6) of the determined values of test of sample for precision was less than 5.0%. Test for recovery was made by the standard addition method, giving results in the range of 80.7%-94.4%. This method was used to analyze 13 actual imported diluted asphalt samples, the benzoapyrene were all determined, and the detection amounts were in the range of 0.816 5-5.356 mg·kg
-1.