AUTOMATIC SOXHLET EXTRACTION

http://www.cyberlipid.org/extract/extr0010.htm

The method described by Soxhlet in 1879 is the most commonly used

example of a semi-continuous method applied to extraction of lipids from
foods. According to the Soxhlet's procedure, oil and fat from solid
material are extracted by repeated washing (percolation) with an organic
solvent, usually hexane or petroleum ether, under reflux in a special
glassware.

In this method the sample is dried, ground into small particles and
placed in a porous cellulose thimble. The thimble is placed in an
extraction chamber (2), which is suspended above a flask containing the
solvent (1) and below a condenser (4). The flask is heated and the solvent
evaporates and moves up into the condenser where it is converted into a
liquid that trickles into the extraction chamber containing the sample. The
extraction chamber is designed so that when the solvent surrounding the
sample exceeds a certain level it overflows and trickles back down into
the boiling flask. At the end of the extraction process, which lasts a few
hours, the flask containing the solvent and lipid is removed. In some
device a funnel (3) allows to recover the solvent at the end of the
extraction after closing a stopcock between the funnel and the extraction
chamber. The solvent in the flask (1) is then evaporated and the mass of
the remaining lipid is measured. The percentage of lipid in the initial sample can then be
calculated.

Despite disadvantages of this procedure (poor extraction of polar lipids, long time
involved, large volumes of solvents, hazards of boiling solvents), several methods
involving automatic solvent extraction were described. Different automated or semi-
automated extraction instruments may be found on the market.

Several solvent extraction systems based on the Soxhlet device are on the market to allow
fast and safe determination of total lipids in food, soil, ....

As an example, FOSS has launched several types of "Soxtec Systems" including

automated or semi-automated analyzers, which extract lipids rapidly and accurately.
These instruments perform boiling, rinsing and solvent recovery. Similarly, Soxtherm
extractors from Gerhardt GmbH was developed to reduce extraction times.
The sample to be analyzed is weighed into cellulose thimbles and inserted in the
extraction device. Except diethyl ether, all solvents may be used (about 15 ml per
sample), with a 75% recovery of the solvent after the extraction which is completed in 30
to 60 min, depending on the application.
Another device by ViscoALPHA enables the user to have a 2, 4 or 6 place system in 2
versions (micro or macro). An electronic unit can control and monitor up to 4 extraction
units individually.
Compact and simple systems with one to six samples are sold by Behr Labor-Technic
GmbH.

The Büchi Extraction System B-811 is an automated system which can be used to
perform an extraction according to the original Soxhlet principle. Four different
extraction methods are possible without making any changes to the unit : Soxhlet
standard, Soxhlet warm, hot extraction and continuous extraction. The system has an
inert gas supply to avoid oxidation during extraction and to accelerate the evaporation
and drying process even with high boiling point solvents (up to 150°C). Several
application notes may be downloaded from the Büchi site.
A comparison of different extraction methods for total lipid quantification in meat and
meat products was reported (Perez-Palacios T et al., Food Chem 2008, 110, 1025). The
Soxhlet method with previous acid hydrolysis had the same efficiency as that of the
method described by Folch.
A microwave-assisted Soxhlet extraction of seed oil (sunflower, soybean, rape) was
described using a cellulose cartridge placed into a quartz extraction vessel inserted in a
modified Microdigest 301 device (Prolabo). This procedure is slightly different from that
described for the extraction of dry materials. Despite a 3 h analysis, the time reduction
and the lack of need for seed grinding makes this procedure a suitable competitor of the
previously described methods (Garcia-Ayuso LE et al., Anal Chem 1998, 70, 2626;
Garcia-Ayuso LE et al., Chromatographia 2000, 52, 103). Comparative experiments have
shown that no significant differences between the extract obtained by the Folch reference
method without fat alterations and the microwave-assisted Soxhlet extraction were
detected. These results demonstrated the applicability of that method for the extraction
step in routine analysis of a great quantity of food samples (Ruiz-Jimenez J et al., Anal
Chim Acta 2004, 525, 159).
This extraction technique, called microwave-assisted Soxhlet extraction, uses two sources
of energy, namely microwaves, applied on the extraction chamber of a modified Soxhlet,
and electrical heating applied on the distillation flask. This system has been used for the
determination of oil content and fatty acid composition of various biological materials
and foodstuffs. To overcome some limitations of the analytical process (water content), a
new and convenient process was designed and developed (Virot M et al., J Chromatogr A
2007, 1174, 138; Virot M et al., J Chromatogr A 2008, 1196-1197, 57).
A modification of that extraction procedure was proposed taking into account the use of a
"green solvent", limonene, instead of hexane (Virot M et al., J Chromatogr A 2008, 1196-
1197, 147). The proposed method is effective and valuable since no significant
difference was obtained when using hexane or limonene for the extraction of oleaginous
seeds.