Analysis of polycyclic aromatic hydrocarbons in soil and sediment with on-line coupled pressurised hot water extraction, hollow fibre microporous membrane liquid–liquid extraction and gas chromatography

The Analyst ◽  
2003 ◽  
Vol 128 (5) ◽  
pp. 434-439 ◽  
Author(s):  
Kati Kuosmanen ◽  
Tuulia Hyötyläinen ◽  
Kari Hartonen ◽  
Marja-Liisa Riekkola
2005 ◽  
Vol 88 (4) ◽  
pp. 1247-1254 ◽  
Author(s):  
Sandra Martinez-López ◽  
Asuncion Morales-Noé ◽  
Agustin Pastor-Garcia ◽  
Angel Morales-Rubio ◽  
Miguel de la Guardia

Abstract The determination of 15 polycyclic aromatic hydrocarbons (PAHs) in olive oil samples has been improved in order to obtain a fast methodology with a low limit of detection through the combination of liquid–liquid extraction with acetonitrile and preparative gel permeation chromatography (GPC) prior to the injection of purified extracts into a C18 column. Acetonitrile–water was used as the mobile phase with a gradient from 50 to 95%, w/w, acetonitrile in 30 min. The oven temperature was maintained at 15°C, and fluorometric detection was made at a fixed excitation wavelength of 264 nm and variable, optimal emission wavelength for each analyte ranging from 352 nm for 11-H-benzo(b)fluorene to 500 nm for indeno(1,2,3-cd)pyrene. Recovery for all the compounds studied varied from 75 to 111%, and limit of detection values from 0.05 ng/g for benzo(k)fluoranthene to 0.48 ng/g for indeno(1,2,3-cd)pyrene, corresponding to 0.09 ng/g benzo(a)pyrene. Results were compared with those obtained by liquid–liquid extraction followed by a cleanup on silica and a direct GPC treatment of oil samples diluted in dichloromethane, 2 other methodologies that are appropriate for quantifying PAHs in olive oils. However, the proposed method improves the determination limits, reduces the time of analysis, and provides a highly stable baseline for sample chromatograms.


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