Comprehensive comparison of classic Soxhlet extraction with Soxtec extraction, ultrasonication extraction, supercritical fluid extraction, microwave assisted extraction and accelerated solvent extraction for the determination of polychlorinated biphenyls in soil

2005 ◽  
Vol 1090 (1-2) ◽  
pp. 1-9 ◽  
Author(s):  
Sune Sporring ◽  
Søren Bøwadt ◽  
Bo Svensmark ◽  
Erland Björklund
1996 ◽  
Vol 79 (1) ◽  
pp. 142-156 ◽  
Author(s):  
Viorica Lopez-A Vila ◽  
Richard Young ◽  
Nataly Teplitsky

Abstract Microwave-assisted extraction (MAE), Soxhlet, soni cation, and supercritical fluid extraction (SFE) were compared in their ability to extract 95 compounds listed in U.S. Environmental Protection Agency Method 8250. Freshly spiked soil samples and 2 standard reference materials were extracted with hexane-acetone (1 + 1) by MAE and Soxhlet extraction, with methylene chloride-acetone (1 + 1) by sonication extraction, and with supercritical carbondioxide modified with 10% methanol by SFE. Results indicate that MAE is a promising extraction technique. Of 94 compounds for which we are reporting data, 51 compounds gave MAE recoveries of >80%; 33,50-79%; 8,20-49%; and 2, <19%. Soxhlet extraction gave very similar results: 50 recoveries were >80%; 32,50-79%; 8,20-49%; and 4, <19%. Sonica tion recoveries were slightly higher: 63 values were >80%; 25,50-79%; 4,20-49%; and 2, <19%. SFE recoveries were the lowest: 37 values were >80%; 37, 50-79%; 12,20-49%, and 8, <19%. MAE gave the best precision: relative standard deviations (RSDs) were <10% for 90 of 94 compounds. Soxhlet extraction gave the worst precision: only 52 of 94 samples gave RSDs ≤10%. Although MAE looks promising, 15 polar basic compounds extracted at 115°C with hexane acetone for 10 min (1000 W power) gave poor recoveries. Because no technique gave acceptable recoveries for these polar compounds, we investigated their extraction with MAE using acetonitrile at 50° and 115°C. Ten of the 15 compounds were quantitatively recovered (>70%) with acetonitrile at 115°C.


2008 ◽  
Vol 91 (5) ◽  
pp. 1124-1129 ◽  
Author(s):  
Takamitsu Otake ◽  
Yoshie Aoyagi ◽  
Masahiko Numata ◽  
Takashi Yarita

Abstract The efficiency of microwave-assisted extraction (MAE) was evaluated for the analysis of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in fish. An isotope dilution method was used for quantification via analysis of the samples by gas chromatography and mass spectrometry. MAE solvent, temperature, and time were optimized, and observed concentrations were compared. The MAE results were also compared to those of other extraction techniques (Soxhlet extraction, pressurized liquid extraction, saponification, and homogenization). Concentrations of PCBs and OCPs obtained by MAE at 120C for 10 min were comparable to those by the other techniques. The results suggest that MAE can be used for the analysis of PCBs and OCPs in fish.


2000 ◽  
Vol 83 (6) ◽  
pp. 1334-1344 ◽  
Author(s):  
Marion Weichbrodt ◽  
Walter Vetter ◽  
Bernd Luckas

Abstract Focused open-vessel microwave-assisted extraction (FOV–MAE), closed-vessel microwave-assisted extraction (CV–MAE), and accelerated solvent extraction (ASE) were used for extraction before determination of organochlorine compounds (polychlorinated biphenyls, DDT, toxaphene, chlordane, hexachlorobenzene, hexachlorocyclohexanes, and dieldrin) in cod liver and fish fillets. Wet samples were extracted without the time-consuming step of lyophilization or other sample-drying procedures. Extractions were performed with the solvent mixture ethyl acetate–cyclohexane (1 + 1, v/v), which allowed direct use of gel-permeation chromatography without solvent exchange. For FOV–MAE, the solvent mixture removed water from the sample matrix via azeotropic distillation. The status of water removal was controlled during extraction by measuring the temperature of the distillate. After water removal, the temperature of the distillate increased and the solvent mixture became less polar. Only the pure extraction solvent allowed quantitative extraction of the organochlorine compounds. For CV–MAE, water could not be separated during the extraction. For this reason, the extraction procedure for wet fish tissue required 2 extraction steps: the first for manual removal of coextracted water, and the second for quantitative extraction of the organochlorine compounds with the pure solvent. Therefore, CV–MAE is less convenient for samples with high water content. For ASE, water in the sample was bound with Na2SO4. The reproducibility for each technique was very good (relative standard deviation was typically <10%); the slightly varying levels were attributed to deviations during sample cleanup and the generally low levels.


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