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Journal of Chromatography A
Volume 1114, Issue 2, 12 May 2006, Pages 198-204
ExTech 2005 - 7th International Symposium on Advances in Extraction Technologies
 
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doi:10.1016/j.chroma.2006.03.110    How to Cite or Link Using DOI (Opens New Window)
Copyright © 2006 Elsevier B.V. All rights reserved.

Analysis of polycyclic aromatic hydrocarbons in pine needles by gas chromatography–mass spectrometry Comparison of different extraction and clean-up procedures

Nuno Ratolaa, Sílvia Lacorteb, Corresponding Author Contact Information, E-mail The Corresponding Author, Arminda Alvesa and Damià Barcelób

aLEPAE, Departamento de Engenharia Química, Faculdade de Engenharia da Universidade do Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal bDepartment of Environmental Chemistry, IIQAB-CSIC, c/Jordi Girona 18-26, 08034 Barcelona, Catalonia, Spain

Available online 18 April 2006.

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Abstract

Three extraction methodologies (Soxhlet, ultrasonic and pressurized liquid extraction) and several clean-up procedures (Florisil, silica and alumina in cartridges or glass column format) were tested and compared to extract 16 US Environmental Protection Agency (EPA) polycyclic aromatic hydrocarbons (PAHs) from Pinus pinea L. needles. Quantification was done by gas chromatography with mass spectrometry, by internal standard method using five deuterated PAH surrogate standards. Among the several extraction and clean-up procedures tested, ultrasonic extraction followed by alumina cartridge clean-up was the preferred method, yielding recoveries between 72 and 100% and limits of detection between 0.22 and 0.71 ng/g dry weight. The performance of the method was tested to determine PAHs in naturally contaminated samples.

Keywords: Polycyclic aromatic hydrocarbons; Pine needles; Soxhlet; Ultrasonic extraction; Pressurized liquid extraction

Article Outline

1. Introduction
2. Experimental
2.1. Chemicals and reagents
2.2. Pine samples; extraction; clean-up
2.2.1. Soxhlet extraction
2.2.2. Ultrasonic extraction
2.2.3. Pressurized liquid extraction
2.2.4. Clean-up
2.2.5. Naturally contaminated samples
2.3. Instrumental analysis
3. Results and discussion
3.1. Preliminary tests on pine needles
3.2. GC–MS conditions and quality parameters
3.3. Extraction and cartridge clean-up of pine needles
3.3.1. Glass columns clean-up
3.4. Versatility of ultrasonic extraction with alumina cartridges clean-up
3.5. Pilot study of pine needles in the Iberian peninsula
4. Conclusions
Acknowledgements
References





Journal of Chromatography A
Volume 1114, Issue 2, 12 May 2006, Pages 198-204
ExTech 2005 - 7th International Symposium on Advances in Extraction Technologies
 
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