Appli cat i on N ote 3 2 5

Extraction of Oils from Oilseeds by

Accelerated Solvent Extraction
David Knowles and Bruce Richter
Thermo Fisher Scientific, Salt Lake City, UT, USA

Introduction Solvents
Accelerated solvent extraction is an extraction method that • Petroleum ether (pesticide quality or equivalent)
signiicantly streamlines sample preparation. A commonly
used solvent is pumped into an extraction cell containing Dionex ASE 200 Accelerated Solvent Extractor Conditions
the sample, which is then brought to an elevated tempera- Oven Temperature: 105 °C
ture and pressure. Minutes later, the extract is transferred Pressure: 6.67 MPa (1000 psi)
from the heated cell to a standard collection vial for
Oven Heatup Time: 5 min
cleanup or analysis. The entire extraction process is fully
automated and performed in minutes for fast and easy Static Time: 10 min
extraction with low solvent consumption. Flush Volume: 100%

Oils for foods and cooking are derived from oilseeds like Purge Time: 60 s
canola, soybeans, corn, lax, cotton, etc. The production of Solvent: Petroleum ether
oil from oilseeds is an important business, and agrono- Static Cycles: 3
mists are continuing to investigate ways to improve the oil
output of the seeds as well as ways to control the compo- It may be necessary to perform three complete extractions
sition of the oil itself. of each sample and combine the results from each
extraction. If the samples contain unsaturated fats that
A common method used to remove the oil from the may be oxidized during extraction, and these fats are to
oilseeds is solvent extraction. Existing solvent extraction be analyzed, the solvent should be degassed to avoid
methods use large volumes of solvent (typically several potential oxidative degradation.
hundred milliliters) and long extraction times (8–16 h) to
remove the oil from the seeds. Once the oil is removed, the Sample Preparation
weight percent of oil in the seeds can be determined, and It is important to reduce the particle size of all samples
the composition of the oils can be studied. by grinding or another appropriate procedure. The
particle diameter should be less than 3 mm. Samples
Accelerated solvent extraction is a relatively new extrac-
should also be mixed with an inert iller such as clean
tion technique that uses elevated temperature and pressure
sand to prevent sample compaction during extraction. Wet
to expedite the removal of analytes from various matrices.
samples (>10 wt%) should be dried in an oven at 105 °C
It is accepted by the U.S. EPA as Method 3545 for
for at least 2 h or mixed with a desiccant such as Thermo
environmental samples, and it has been applied to other
Scientiic™ Dionex™ ASE Diatomaceous Earth Dispersant
sample extraction areas. Accelerated solvent extraction
P/N 062819, (1:1 w/w) prior to extraction. Depending on
can be used to extract a 10 g sample in about 14 min with
the density of the samples, it may be necessary to use the
a total solvent consumption of approximately 16 mL.
22 mL cells.
The procedures described in this application note apply to
the determination of oil content in oilseeds. The oil
content is determined by collecting the extracts in
preweighed vials, evaporating the solvent with a nitrogen
stream and reweighing the vials.

Equipment
• Thermo Scientiic™ Dionex™ ASE™ 200 Accelerated
Solvent Extractor equipped with 11 or 22 mL cells
• Analytical balance
• Vials for collection of extracts (40 mL, P/N 49465;
60 mL, P/N 49466)
2 Procedure 100
Grind the sample to an appropriate particle size (less than
2 to 3 mm diameter). Place a cellulose disk at the outlet 80
end of the extraction cell. Weigh out 3 to 10 g of sample
in a beaker. Mix with Dionex ASE Diatomaceous Earth 60
Percent
Dispersant if the sample is wet. If not, mix with sand Extracted
40
(approximately 1:1) and load into the extraction cell. Fill
any void volume with clean sand.
20
Place closed cells into upper carousel with the appropriate
number of clean, preweighed collection vials. (It is best to 0
240 360 480
weigh the vials without the lids and septa before extrac- Minutes
tion and then again after solvent evaporation to eliminate
Figure 1. Extraction of oil from oilseeds: FOSFA.
any contribution caused by the loss of material from the
lids or septa.) Set the method conditions on the Dionex
100
ASE 200 Accelerated Solvent Extractor system and initiate
the run.
80
Upon completion of the extraction, place the collection
vials in an evaporator with nitrogen to evaporate the 60
Percent
solvent. Then, weigh the residue to determine the percent Extracted
40
of oil in the original sample.

Discussion and Results 20

The example used here is of canola seeds which contain
0
approximately 45 wt percent oil. In order to understand 30 60 90
the advantages of accelerated solvent extraction, it is Minutes
important to understand the currently used extraction Figure 2. Extraction of oil from oilseeds: accelerated solvent extraction.
methodology. The method currently used is speciied as
AOCS (American Oil Chemist Society) Oficial Method
AM 2-93 which is based on the FOSFA (Federation of Oil 1.2
Seeds and Fat Association) Oficial Method. The speciics 1.0
of this method are given in Table 1.
0.8
Rate 0.6
Table 1. AOCS Method AM 2–93.
(g/h)
Sample Size 4 g ground seeds 0.4

Oven 130 °C, 2 h 0.2

Extract 4 h, drain solvent and cool 0
Regrind 7 min FOSFA Accelerated Solvent Extraction

Extract 2 h, drain solvent and cool Figure 3. Rate of oil extraction from oilseeds.
Solvent Petroleum ether
Total Volume Solvent Used 150–250 mL Studies were performed to determine the effect of the
Total Time 10.5 h elevated temperatures on the triglycerides during the
extraction by accelerated solvent extraction. Two values,
peroxide value (PV) and free fatty acid (FFA), were
There are several ways to compare the performance of determined for oils that had been extracted at different
accelerated solvent extraction against that of the standard temperatures. The resulting data are given in Table 2.
method. First, the weight percent of oil in the seeds was
determined to be 44.9% with 0.31% RSD (n = 3) as
Table 2. Peroxide values (PV) and free fatty acid (FFA) profiles on grain extracts
compared to 45.2% with 0.24% RSD (n = 12) for the
obtained by accelerated solvent extraction with petroleum ether.
AOCS method. Second, the percent of the total oil
extracted as a function of time can be compared for the Extraction Temp. PV FFA
two techniques (see Figures 1 and 2). Third, the weight of (°C) (µg/L or ppm) (%)
oil extracted per unit time can be contrasted for acceler- 50 2.24 0.57
ated solvent extraction and the FOSFA procedure (see
70 3.15 0.80
Figure 3). As can be seen, accelerated solvent extraction
gives comparable results faster and with less solvent 110 3.23 1.05
usage. 130 2.08 1.28
The PV is a measure of the oxidation of the triglycerides,
and any value less than 5 ppm shows no signiicant
oxidation as compared to Soxhlet. The FFA is a measure-

Appli cat i on N ote 3 2 5

ment of triglyceride degradation, and typical values from
Soxhlet are 0.5–1.0%. These data show that no signiicant
oxidation or triglyceride degradation occurs during
accelerated solvent extraction

Conclusion
The data presented here have demonstrated that acceler-
ated solvent extraction can be used to extract and
determine the oil content of oilseeds. The data generated
are equivalent to those obtained by existing methods, but
the time and solvent usage are signiicantly less with
accelerated solvent extraction.

Acknowledgements
The peroxide values and free fatty acid contents were
provided by the Grain Research laboratory, Canadian
Grain Commission, Winnipeg, Manitoba.

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