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    超声提取-真空离心浓缩-超高效液相色谱法测定PM2.5中16种多环芳烃的含量

    Determination of 16 Polycyclic Aromatic Hydrocarbons in PM2.5 by Ultra-High Performance Liquid Chromatography with Ultrasonic Extraction and Vacuum Centrifugal Concentration

    • 摘要: 将处理后的滤膜置于大流量颗粒物采样器中以采样速率800 L·min−1连续采样22 h,将该滤膜平均分割成8份,取其中一份剪碎后置于50 mL离心管中,加入15 mL乙腈,涡旋30 s,于20 ℃超声提取30 min,离心10 min,再加入10 mL乙腈重复提取1次,合并2次提取液,过0.45 μm滤膜,于50 ℃真空离心浓缩至近干,用乙腈定容至1.0 mL,混匀,过0.45 μm滤膜,采用超高效液相色谱法测定滤液中16种多环芳烃的含量。以Agilent Eclipse PAH RRHD色谱柱为固定相,以不同体积比的水-乙腈混合溶液为流动相进行梯度洗脱。结果表明,16种多环芳烃的质量浓度在0.02~1.0 mg·L−1内与对应的峰面积呈线性关系,检出限(3s)为0.003~0.033 ng·m−3。按照标准加入法进行回收试验,回收率为80.8%~111%,测定值的相对标准偏差(n=8)为2.6%~7.1%。方法用于某监测点全年PM2.5样品的分析,不同季节下16种多环芳烃的检出总量为0.52~2.53 ng·m−3,检出总量由大到小依次为冬季、秋季、春季、夏季。

       

      Abstract: The treated filter membrane was placed in a high-flow particulate matter sampler for continuous sampling for 22 h at a flow rate of 800 L · min−1. The filter was cut into 8 equal pieces, one of which was shredded and placed in a 50 mL- centrifuge tube. 15 mL of acetonitrile was added, and the mixture was vortexed for 30 s, ultrasonic extracted for 30 min at 20 ℃ and centrifugated for 10 min. 10 mL of acetonitrile was added and the extraction was repeated once. The two extraction solutions were combined and filtered through 0.45 μm filter membrane, and the filtrate was concentrated to near dryness by vacuum centrifugation at 50 ℃. The solution was diluted to 1.0 mL with acetonitrile and mixed well. The solution was passed through 0.45 μm filter membrane, and 16 polycyclic aromatic hydrocarbons in the filtrate were determined by ultra-high performance liquid chromatography. Agilent Eclipse PAH RRHD chromatographic column was used as the stationary phase and the mixed solution composed of water and acetonitrile at different volume ratios was used as the mobile phase for gradient elution. As shown by the results, linear relationships between the corresponding peak areas and mass concentrations of 16 polycyclic aromatic hydrocarbons were kept in the range of 0.02-1.0 mg · L−1, with detection limits (3s) in the range of 0.003-0.033 ng · m−3. Test for recovery was made by the standard addition method, giving results in the range of 80.8%-111%, with RSDs (n=8) of the determined values in the range of 2.6%-7.1%. This method was used for analysis of annual PM2.5 samples at a monitoring site. The total detection amounts of the 16 polycyclic aromatic hydrocarbons in different seasons were in the range of 0.52-2.53 ng · m−3, and the total detection amounts decreased in the order of winter, autumn, spring, and summer.

       

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