Microwave-assisted extraction versus Soxhlet extraction for the analysis of short-chain chlorinated alkanes in sediments

Abstract

Microwave-assisted extraction (MAE) was evaluated as a possible alternative to Soxhlet extraction for analysing short-chain chlorinated alkanes (commonly called short-chain chlorinated paraffins, SCCPs) in river sediment samples, using gas chromatography coupled to negative chemical ionisation mass spectrometry. For MAE optimisation, several extraction parameters such as solvent extraction mixture, extraction time and extraction temperature were studied. Maximum extraction efficiencies for SCCPs (90%) and for 12 polychlorinated biphenyl (PCB) congeners (91-95%) were achieved using 5 g of sediment sample, 30 ml of n-hexane-acetone (1:1, v/v) as solvent extraction, and 15 min and 115 degrees C of extraction time and temperature, respectively. Activated Florisil was used to clean-up the extracts, allowing highly selective separation of SCCPs from other organic contaminants such as PCBs. MAE was compared with a conventional extraction technique such as Soxhlet and good agreement in the results was obtained. Quality parameters of the optimised MAE method such as run-to-run (R.S.D. 7%) and day-to-day precision (R.S.D. 9%) were determined using spiked river sediment samples, with LODs of 1.5 ng g(-1). This method was successfully applied to the analysis of SCCPs in river sediment samples at concentrations below the ng g(-1) level. O 2004 Elsevier B.V. All rights reserved.

Microwave-assisted extraction versus Soxhlet extraction to determine triterpene acids in olive skins

“…MAE is also one of the best green technologies and has emerged as an efficient method for extracting several natural products, contaminants, additives, etc. [17][18][19][20][21][22][23]. In recent years, MAE has been applied to the extraction of several types of compounds, such as phenolic products from alperujo [24], additives in polyolelfins and polymers [25], diterpenes in green coffee oil [26], triterpenes and biophenols in olive leaves [27][28][29][30], polychlorinated biphenyls in foods and soils [31], and oleanolic acid (OA) in Lantana camara [32].…”

Presence of Chlorinated Paraffins in Sediments from the North and Baltic Seas

“…However, recent publications showed that LRMS can be used (Castells et al 2004;Zencak et al 2005). This requires an efficient sample clean-up (Parera et al 2004;Reth et al 2005) and a special approach to eliminate interferences by mass overlap .…”

“…SCCP concentrations between 24 and 46 ng/g dry weight were determined in freshwater sediments for a background area in the Czech Republic and between 5 and 181 ng/g for two areas influenced by industry (Stejnarova et al 2005). Levels of SCCPs in river sediments were in the range of 250 ng/g to 3260 ng/g in Spain (Parera et al 2004).…”

Study of polycyclic aromatic hydrocarbon contamination in sediments and northern waters Lebanon: Rivers, transition zones and port sites.

“…La méthode d'extraction assistée par micro-onde utilisée pour l'extraction des sédiments a été adaptée des méthodes validées décrites par David et al (2009), Kinani et al (2010) et Parera et al (2004) pour l'extraction des polluants organiques dans des sédiments (5 ± 0,5 g/extraction -fraction < 2 mm) lyophilisés et broyés. Cette technique consiste à extraire des contaminants organiques d'une matrice solide par un ou des solvants organiques portés à haute température et haute pression.…”