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    高效液相色谱法测定进口稀释沥青中苯并a芘的含量

    Determination of Benzoapyrene in Imported Diluted Asphalt by High Performance Liquid Chromatography

    • 摘要: 取样品0.05 g置于50 mL离心管中,加入10 mL正己烷,超声20 min,离心10 min,取上清液置于另一50 mL离心管中,残渣用正己烷重复提取一次,合并上清液,于40 ℃氮气吹至2~3 mL,过Macklin层析硅胶自制层析柱净化,加入70 mL正己烷淋洗,淋洗液于40 ℃氮气吹至2 mL,过Agela Cleanert Bap-3萃取柱(用5 mL二氯甲烷和5 mL正己烷活化),加入10 mL正己烷(每次5 mL)淋洗,5 mL二氯甲烷洗脱,洗脱液于40 ℃氮吹至近干,加入1.0 mL乙腈,涡旋振荡0.5 min,过0.22 μm有机滤膜,滤液供高效液相色谱仪分析。以Waters PAH C18色谱柱为固定相,以不同体积比的乙腈-水混合液为流动相进行梯度洗脱。结果表明,苯并a芘的质量浓度在5.00~500.0 μg·L-1内与对应的峰面积呈线性关系,检出限(3S/N)为10 μg·kg-1。样品精密度试验所得测定值的相对标准偏差(n=6)小于5.0%,按照标准加入法进行回收试验,回收率为80.7%~94.4%。方法用于13份实际进口稀释沥青样品的分析,均检出苯并a芘,检出量为0.816 5~5.356 mg·kg-1

       

      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 C18 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.

       

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