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| Determination on Ultra-trace of Polycyclic Aromatic Hydrocarbons in Atmospheric Particulate Matters by Liquid Chromatography Coupled with Ultrasonic Extraction and Online Solid Phase Extraction Concentration |
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| DOI： |
| KeyWord:atmospheric particulate matters polycyclic aromatic hydrocarbons(PAHs) liquid chromatography(LC) ultrasonic extraction online solid phase extraction(online SPE) fluorescence detection |
| Author | Institution |
| HUANG Zhao-zhang，WANG Chao，QI Wei-hong，CHEN Ye，YUAN Mao |
1. China National Environmental Monitoring Centre， Beijing ， China; 2. Guangzhou Environmental Monitoring Centre， Guangzhou ， China; 3. Handan Environmental Monitoring Centre， Handan ， China |
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| Abstract: |
| A liquid chromatography(LC) with ultrasonic extraction and online solid phase extraction(online SPE) concentration was developed for the determination of 15 polycyclic aromatic hydrocarbons(PAHs) in atmospheric particulate matters. Through the optimization of instrument analysis， sample extraction and preparation， and elimination of ion interference, the best experimental conditions were obtained. A slice of 1.4 cm2 was cut from a particulate filter membrane sample， and extracted with 2 mL acetonitrile by ultrasonic extration for 10 min. The extract was high-speedily centrifugated to remove the suspended particles， then prepared as an solution containing 25% (by volume) acetonitrile. 2 mL of the prepared solution was directly injected into the online SPE/LC. Online purification and enrichment of the samples were carried out on an Acclaim Polar Advantage Ⅱ C18 SPE column(50 mm × 4.6 mm， 3 μm). 15 PAHs were separated on a Hypersil Green PAH column(150 mm × 3 mm, 3 μm) with 0.05 mol/L ammonium acetate solution－acetonitrile as mobile phase， and detected by fluorescent detector. The linear correlation coefficients of the 15 PAHs were greater than 0.992. Calculated by air volume of 23 m3 and filter membrane area of 12 cm2， the limits of detection(LOD) of the method were in the range of 0.03 × 10－3－33.27 × 10－3 ng/m3 ， in which the LOD for benzo(a)pyrene(B(a)P) was 0.67 × 10－3 ng/m3. The recoveries for 15 PAHs at two spiked levels of 40 ng/L and 200 ng/L were in the ranges of 91.4%－126% and 103%－123%， with relative standard deviations(RSD， n=6) of 4.4%－10% and 5.2%－12%， respectively. The method is simple， sensitive and low sample consumptive(1.4 cm2)， and could meet the requirements for analysis of ultra-trace PAHs in atmospheric particulate matters. |
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