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need help for new rue extractions Options
 
Jox
#1 Posted : 7/11/2013 3:16:49 AM
Hi all,

I found this article, it is in pdf form.

If there is a chemist to kind of simplify this, but it seems that its easier then the teks we have for the rue.

this is the main part:

Three different extraction
procedures were used in order to obtain
harmala alkaloids from Syrian Rue seeds.
The thr
ee methods of extraction involve both
the acidification of the alkaloids, followed by
the removal of impurities with organic
solvent, and basification of the solution
followed by the extraction of the alkaloids
with the organic solvent. The first extracti
on
involved the use of chloroform and sodium
hydroxide, the second ethyl acetate and
sodium bicarbonate, and the third ethyl
acetate and sodium hydroxide. The
extraction method was based on a
previously developed method [4].
For each extraction, approxim
ately
10g of Syrian Rue seeds were used. The
seeds were ground to a fine powder using a
coffee grinder and placed in a clean, dry
beaker. To the beaker was added five times
the weight of the seeds in milliliters
(approximately 50mL) of an acetic acid
sol
ution. The solution contained 30g of
acetic acid per liter of water. The mixture
was placed on a stir plate for five minutes at
a low speed. Following the five minutes, the
solid material was removed using a filter
system with a Bucher funnel lined with
Whatman 4 filter paper. During the filtering
process, the plant material was washed
twice with the aforementioned acetic acid
solution (each wash was approximately
10mL).
After the plant material was filtered,
50mL of petroleum ether and 50mL of ethyl
acetate were added to a separatory funnel
along with the resulting solution from the
plant material and acetic acid solution in
order to remove any organic impurities. The
solution was gently mixed by way of
inversion and the aqueous layer was
removed fo
r later use. Leaving the top layer
in the separatory funnel, and addition 50mL
of petroleum ether and 50mL of ethyl
acetate was added, mixed, and again the
aqueous layer was removed. This process
was repeated once more for a total of three
times.
To the saved aqueous solution, an aqueous
base was added drop wise until the solution
turned basic. After every five to ten drops
had been added, the solution was stirred
and the basicity was tested using pH paper.
When the transformation had occurred, t
he
pH paper turned blue in color and the
solution went from being a transparent
brown color to a cloudy, light brown color.
Finally, 100mL of the organic
solvent was added to the separatory funnel
along with the now basic solution. The
contents of the
funnel were mixed gently by
inversion and the layer containing the
organic solvent was collected. To the
solution still in the funnel, an additional
100mL of the solvent was added and the
organic solvent layer was again collected.
This was repeated one
more time, for a total
of three total extractions. After the final
collection, sodium sulfate was added to the
solution in order to remove any excess
water. (It is not important to add a specified
amount of sodium sulfate to the solution;
when the sodiu
m sulfate ceases to clump,
this is an indication that the water has been
removed.) The now dry solution was poured
through a glass funnel, using cotton as a
filter, into a preweighed 500mL round
bottom flask. The cotton ball was washed
with approximately
5mL of the organic
solvent to ensure that all of the extract was
contained in the round bottom flask. After
the filtration, the solvent was removed from
the solution using rotary evaporation using
an aspirator. For further drying, a low
pressure pump wa
s used to pump out any
remaining solvent. After the pumping
process was finished, the flask was weighed
to obtain a yield.
For the first extraction, the organic
solvent used was chloroform and the
aqueous base was 1M NaOH. In this
procedure, 10.0768g of
Syrian Rue seeds
were used. The second extraction involved
the organic solvent ethyl acetate and the
aqueous base sodium bicarbonate. In this
procedure, 10.0743g of Syrian Rue seeds
were used. In the third and final extraction,
the organic solvent used
was ethyl acetate
and the aqueous base was 1M NaOH. In
this procedure, 9.9929g of Syrian Rue seeds
were used
 
 
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