The Malaysian Journal of Analytical Sciences Vol 12 No 2 (2008): 352 – 356

 

 

 

SELECTIVE ACCELERATED SOLVENT EXTRACTION FOR THE ANALYSIS OF SOIL POLYCYCLIC AROMATIC HYDROCARBONS AND STEROLS

 

Rozita Osman1*, Nor’ashikin Saim1, and Md Pauzi Abdullah2

 

1Faculty of Applied Sciences, Universiti Teknologi MARA 40450 Shah Alam, Selangor

2Faculty of Science and Technology,

Universiti Kebangsaan Malaysia 43600 Bangi, Selangor, Malaysia

 

*Corresponding author: rozit471@salam.uitm.edu.my

 

Abstract

Accelerated solvent extraction (ASE) has been successfully used in the analysis of a wide range of chemicals from many sample matrices. However, the main problem with accelerated solvent extraction is low selectivity towards the analyte because during the extraction process, many interfering components are co-extracted together with target analytes and thus requires post-extraction clean-up processes. In this study, a selective accelerated solvent extraction with clean-up step incorporated inside the extraction cell was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) and sterols in soil. PAHs (naphthalene, acenaphtene, anthracene, pyrene) and sterols (coprostanol, cholesterol, stigmasterol, stigmastanol) were extracted separately using two elution steps. The selectivity and efficiency of this approach were evaluated using several sorbents and proper choice of solvents. Using polar sorbents, PAHs were recovered in the first extraction using n-hexane while sterols were recovered in the second extraction using a more polar solvent such as methanol, isopropanol, acetone and mixture of DCM:MeOH (40:60, v/v). Recoveries for PAHs ranged from 76.5-99.2 % and sterols from 83.7.7-91.4% using silica as the sorbent, n-hexane as the first eluent, and methanol as the second eluent.

 

Keywords: Accelerated solvent extraction, polycyclic aromatic hydrocarbons, sterols.

 

References

1.       Burkhardt, M. R., ReVello, R. C., Smith, S. G., Zaugg, S. D. 2005. Pressurized liquid extraction using water/isopropanol couple with solid-phase extraction cleanup for industrial and anthropogenic waste-indicator compounds in sediment. Analytica Chimica Acta, 534, 89-100.

2.       Björklund, E., Sporring, S., Wiberg, K., Haglund, P., von Holst, C. 2006. New strategies for extraction and clean-up of persistent organic pollutants from food and feed samples using selective pressurized liquid extraction. Trends in Analytical Chemistry, 25, 4, 319-325.

3.       Kiguchi,O., Saitoh, K., Ogawa, N. 2007. Simultaneous extraction of polychlorinated dibenzo-p-dioxins, polychlorinated biphenyl from contaminated soil using pressurized liquid extraction. Journal of Chromatography A, 1144, 262-268.

4.       Ramos, L., Vreuls, J.J., Brinkman, U.A.Th. 2000. Miniaturised pressurized liquid extraction of polycyclic aromatic hydrocarbons from soil and sediment with subsequent large-volume injection-gas chromatography. Journal of Chromatography A, 891, 275-286.

5.       Müller, E., Bjöklund, E., von Holst, C. 2001. On-line clean-up of pressurized liquid extracts for the determination of polychlorinated biphenyls in feedingstuffs and food matrices using gas chromatography-mass spectrometry. Journal of Chromatography A,  925, 197-205.

6.       Sporring,S., Bjöklund, E. 2004. Selective pressurized liquid extraction of polychlorinated biphenyls from fat-containing food and feed samples Influence of cell dimensions, solvent type, temperature and flush volume. Journal of Chromatography A, 1040, 155-161.

7.       Gómez-Ariza, J.L., Giráldez, I., Velasco, A., Morales, E. 2002. Determination of polychlorinated biphenyls in biota samples using simultaneous pressurized liquid extraction and purification. Journal of Chromatography A, 946, 209-219.

8.       Hussen, A., Westbom, R., Megersa,N., Mathiasson, L., Björklund, E. 2007. Selective pressurized liquid extraction for multi-residue analysis of organochlorine pesticides in soil. Journal of Chromatography A,  Article in press.

9.       Sun, F., Littlejohn, D., Gibson, M.D. 1998. Ultrasonication extraction and solid phase extraction clean-up for determination of US EPA 16 priority pollutant polycyclic aromatic hydrocarbons in soils by reversed-phased liquid chromatography with ultraviolet absorption detection.  Analytica Chimica Acta, 364, 1-11.

10.    Concha-Grańa, E., Turnes-Carou, M.I., Muniategui-Lorenzo, S., López-Mahia, P., Fernández-Fernández, E., Prada-Rodriguez, D. 2004. Development of pressurized liquid extraction and cleanup procedures for determination of organochlorine pesticides in soils. Journal of Chromatography A, 1047, 147-155.

11.    Kiguchi, O., Kobayashi, T., Saitoh, K., Ogawa, N. 2006. Pressurized liquid extraction of polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans and coplanar polychlorinated biphenyls from contaminated soil. Journal of Chromatography A, 1108, 176-182.

12.    Flotron, V., Houessou, J., Bosio, A., Delteil, C., Bermond, A., Camel, V. 2003. Rapid determination of polycyclic aromatic hydrocarbons in sewage sludges using microwave-assisted solvent extraction Comparison with other extraction methods. Journal of Chromatography A, 999, 175-184.

13.    Ong, R., Lundstedt, S., Haglund, P., Marriot, P. 2003. Pressurised liquid extraction-comprehensive two-dimensional gas chromatography for fast-screening of polycyclic aromatic hydrocarbons in soil. Journal of Chromatography A, 1019, 221-232.

14.    Kim, J.H., Moon, J.K., Li, Q. X., Cho, J. Y. 2003. One-step pressurized liquid extraction method for the analysis of polycyclic aromatic hydrocarbons. Analytica Chimica Acta, 498, 55-60.

 




Previous                    Content                    Next