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Extraction of atropine from Datura Innoxia using liquid membrane Technique

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 Iraqi Journal of Chemical and Petroleum Engineering
Vol.10 No.1 (March2009) 23-27
Iraqi Journal of Chemical
ISSN: 1997-4884 University of Baghdad
and Petroleum Engineering College of Engineering

Extraction of atropine from Datura Innoxia using liquid membrane

Technique

Adel al-Hemiri* and Wasan O. Noori

*
Chemical Engineering Department - College of Engineering - University of Baghdad – Iraq

Abstract
Selective recovery of atropine from Datura innoxia seeds was studied. Applying pertraction in a rotating film contactor
(RFC) the alkaloid was successfully recovered from native aqueous extracts obtained from the plant seeds. Decane as a
liquid membrane and sulfuric acid as a stripping agent were used. Pertraction from native liquid extracts provided also
a good atropine refinement, since the most of co-extracted from the plant species remained in the feed or membrane
solution. Solid–liquid extraction of atropine from Datura innoxia seeds was coupled with RF-pertraction in order to
purify simultaneously the extract obtained from the plant. Applying the integrated process, proposed in this study, a
product containing 92.6% atropine was obtained.

Keywords: Extraction, Liquid membrane, Pertraction, Atropine, Purification

Introduction alkaloids are recovered in the stripping solutions as

salts. Because of the relatively low distribution
Atropine sulphate is used widely in medicine for coefficients, for a complete recovery of the alkaloids,
resuscitation, anesthesia, ophthalmology, treat peptic both extraction and stripping operations have to be
ulcer and as an antidote for poisoning by repeated at least three to four times.(4) The difference
organophosphate insecticides and nerve gases(1). in pH values between the two aqueous solutions is the
driving force in this case.(5)
Atropine is found in many members of the Solanaceae
family. The most commonly found sources are Atropa One of the modern techniques of mixture separation is
belladonna, Datura innoxia, D. metel, and D. the application of liquid membranes. They reveal the
stramonium. Other sources include members of the ability of selective transport of mixture components in
Brugmansia and Hyoscyamus genera. The Nicotiana which a liquid membrane constitutes a separate phase
genus (including the tobacco plant, N. tabacum) is which separates two other liquid or gas phases. This
also found in the Solanaceae family, but these plants property of membranes makes them useful in the
do not contain atropine or other tropane alkaloids.(2) textile and food industries, in hydrometallurgy,
medicine, biotechnology, environmental protection, in
Atropine can be extracted from the plant as free bases the separation of hydrocarbons and gases, and in the
using basic aqueous solutions or as salts using concentration and separation of amino acids, metal
acidified solutions. The obtained aqueous extracts ions and other mixtures and suspensions.(3) The
contain many undesirable co-extracted species and the alkaloid, atropine, is an organic ester which may be
content of alkaloids is rather low. Usually, the prepared synthetically by combining tropine and
obtained native liquid extracts are purified using tropic acid, but is usually obtained by extraction from
repeatedly performed solvent extraction operations. some Solanaceae plants.(6)
The alkaloids are extracted from basic solutions with
an appropriate organic solvent. Then, the organic This work was conducted to study the process of
solutions are stripped by acidic solutions and the atropine recovery from its solution using a liquid

IJCPE Vol.10 No.1 (March 2009)

Extraction of atropine from Datura Innoxia using liquid membrane technique

membrane technique and to apply this procedure for contains the membrane liquid. Four discs, 0.5mm thick
selective recovery of the alkaloids from native and 0.17m in diameter, mounted vertically on a common
aqueous extraction of Datura innoxia seeds to produce shaft, rotated in each compartment, providing continuous
atropine sulphate. renewal of the aqueous films, covering the discs, as well
as the stirring of all three liquids. The lower part of each
Experimental disc (up to one-third of the disc diameter) is immersed in
the corresponding aqueous solution and the larger, upper
Reagents and analytical methods used part is immersed in the organic membrane liquid, as
Studies of atropine permeation through the liquid shown in (Fig.2). The discs surfaces being hydrophilic,
membrane were carried out using atropine aqueous intended to homogenize the attached aqueous films.
solutions. The atropine was extracted from Datura Hence, the aqueous solutions occupying the lower parts
innoxia seeds (collected in 2004, region of dyala, Iraq) of each compartment form mobile liquid films on the
applying solid–liquid extraction. Decane (99%, BDH) as corresponding disc surfaces, which are in direct contact
a liquid membrane and sulphuric acid (POCH) as a with the common membrane liquid, filling the upper part
stripping agent were used. Ammonia solution (CHEM- of apparatus. The two stages could be connected in a way
SUPPLY, 30%), and sulphuric acid were used to adjust permitting co-, counter-current or batch operation modes.
the acidity of the aqueous solutions. The latter was chosen in our experiments. To homogenize
Atropine concentration in the aqueous solutions was the aqueous solutions and to provide samples from each
measured by UV spectroscopy, λ = 257 nm (λ being the solution, both liquids were re-circulated by means of two
absorbance) and calculated on the basis of atropine peristaltic pumps. A variable rotation speed electric
(hyoscyamine). For this analysis sulphuric acid and motor provided constant shaft rotation.
ammonia, as well as diethyl ether (Fluka AG, Buchs SG), For the pertraction studies, the following three liquid-
heptane (HOPKIN & WILLIAMS), hexane (ALDRICH), phase system was used:
Diiso propyl ether (BDH) were used. Since the amount  feed (donor) solution (F): 250 ml aqueous
of co-extracted species in the acceptor solutions was solution
found to be insignificant, atropine concentration in these  membrane solution (M): 500 ml
solutions was determined directly by UV-spectroscopy,  stripping (acceptor) solution (A): 250 ml
also the acidity of the aqueous solutions was measured by
means of a laboratory pH meter (MAURITUIUS).

Experimental equipment and procedures

The liquid membrane in a rotating film contactor (RFC)
offers more intensive hydrodynamics and therefore, a
faster pertraction process. Pertraction in a RFC is a
special bulk liquid membrane technique in which two
aqueous solutions (feed and stripping solutions) form
mobile films on the surfaces of vertical rotating discs,
partially immersed in the organic membrane liquid. This
pertraction technique provides stable and efficient
continuous operation, avoiding the phase dispersion or
phase intermixing .(7)
The purpose of rotation of hydrophilic discs is to increase
the mass transfer effectiveness, the flow of two crossing
streams produced in the membrane is in such a way that a
vortex flow is achieved. This causes a renewal of the
contact area and considerable intensification of mass
transfer.(8)
Pertraction studies were carried out in a 3000 ml
laboratory rotating film contactor made of Perspex
(Plexiglas®) (Fig.1). The apparatus body contained two
extraction stages of equal volume. The space in the lower
part of each stage is separated into two compartments, for
the feed and stripping solutions, respectively.
Compartments containing the same aqueous solution are
interconnected. The upper part of both compartments Fig. 1 Scheme of Rotating film contactor [4]

24
IJCPE Vol.10 No.1 (March 2009)
 Adel al-Hemiri and Wasan O. Noori

Results and Discussion Effect of pH of the aqueous acceptor solution

From Fig(3), it can be seen that the best results obtained
The results obtained for the extraction of atropine from at pH=2.1 . This is because the atropine must be isolated
Datura innoxia are discussed below. as salt by using dilute acid but if acceptor solution is
more diluted which leads to small amount of (H2SO4)
Effect of type of liquid membrane molecular in acceptor aqueous solution therefore, being
not enough to produce large amount of atropine sulphate.
Figure (2) presents a comparison of the liquid membranes On the other hand when stronger acid is used also gives
used. All five LM to some extent show similar behavior. smaller amount of Atropine sulphate.
During experimentation the white crystals of Atropine
were observed to start forming after about 15 minutes of
operation. 105

From Fig.(2) it can be seen that decane and heptane gave 90

the highest concentration of Atropine after one hour of

Concentraion of Atropine (g/m 3)

75
operation and then the concentration was steady or
60
dropped only slightly.
However, when using heptane the concentration of 45

atropine decreased, after one hour, because the 30

irreversible reaction lead to atropine transport from 15
acceptor solution to feed solution. Therefore, if heptane is 0
to be used the reaction must be stopped after one hour. As 0 20 40 60 80 100 120 140
Time (min)
can be seen that the other solvents (hexane, propyl ether
and ethyl ether) gave lower concentration values and pH=2.1 pH=1.5

there was some loss of these solvents during operation

due to their high volatility, a problem is not encountered Fig.3 Effect pH of acceptor solution
with Decane.
Finally, it should be noted that in the present work decane Effect of amount of seed
and heptane were used (for the first time) along with
other solvents used by earlier workers (viz; Hexane, When doubling the amount of seeds (7.2g instead of
Diiso propyl ether and ethyl ether). And Decane was 3.6g) and keeping the conditions constant. This produced
found to be the best solvent for the duty considered, as higher values of atropine sulphate in comparison with the
shown below. employed half amount of seeds as shown in Fig (4).
Wherewithal these results increased of seeds weight lead
to increased amount of atropine in feed solution in the
same time in membrane as well as in the stripping phase.
105
It is reasonable to observe increases in extraction by
90 increasing the atropine concentration in the feed phase.
This is true for all extraction processes.
75
Concentration of Atropine (g/m3)

60 160
Concentration of Atropine (g/m 3)

140
45
120
30
100
15 80
60
0
40
0 20 40 60 80 100 120 140
Decane Time (min) Heptane 20
Hexane Propyl ether
Ethyl ether 0
0 50 100 150
Time (min)
Fig. 2 Effect of liquid membrane used
Decane (w=3.6)

Fig.4 Effect of amount of seeds

25
IJCPE Vol.10 No.1 (March 2009)
Extraction of atropine from Datura Innoxia using liquid membrane technique

Effect of pH of feed solution

It is observed that the pH of the aqueous donor (feed) solvent Atropine Atropine in Yield %
phase played an important role on the extraction of in feed product gram/
atropine values. From Fig (5) It can be seen that the best gram/ m3 m3
result when pH equal 9.4
Decane (two 130.45 120.855 92.645
stage)
Decane (one 130.45 100.91 77.35
140 stage)
120
Atropine concentration (g/m 3)

Heptane 130.45 95.148 72.94

100

80
Hexane 130.45 31.42 24.086

60 Diiso propyl 130.45 48.116 36.88

40
ether
Ethyl ether 130.45 27.292 20.92
20

0
7 8 9 10 11 12 13
pH of feed solution

Conclusions
Fig.5, Effect pH of feed solution
Pertraction in a rotating film contactor is a suitable
technique for atropine recovery from its solutions,
In addition, the experiments were carried out under the
including native liquid extracts of Datura innoxia . The
best conditions obtained, unless otherwise stated, these
process of atropine recovery from the plant seeds using
conditions are: pH of feed solution 9.4, rpm=10, weight
decane as a liquid membrane is very selective.
of seeds=3.6gm, pH of acceptor solution 2.1 and two
1. The highest atropine yield (92.6%) was achieved
stage unit.
when using two stages.
Yield
2. It was found that the decane is the best solvent as
Datura innoxia contain atropine, hyoscine as well as
small amount of hyoscyamine and other alkaloids. liquid membrane.(12)
Generally the content of alkaloids in Datura is (0.01 - 3
3. Best pH value of acceptor solution is 2.1 and of feed
%) from dry weight, this percentage depended on plant
type, environmental and agriculture process.(9),(10) solution are 9.4.
From Herbal India Constitution the major
4. It was found that the atropine conversion increases
chemical compounds found in Datura innoxia is 33%
atropine, 66% hyoscine and 1% hyoscyamine oxide and with increasing amount of Datura seeds feed.
other compounds.(11)
5. The hydrophilic discs of stainless steel gave good
Therefore the maximum concentration of atropine in
seeds is theoretically (3% * 0.33 * 3.6gram/ 250cm3) extraction.
equal o.1425 * 10-3 (gram/ cm3) = (142.5 gram/m3), but
6. Increasing the number of stages caused increased
from our experiments on the local plant the concentration
was found to be (132.54 gram/m3) atropine extraction.
And the following table shows the amount of atropine in
feed and in product, as well as the yield(12).

26
IJCPE Vol.10 No.1 (March 2009)
 Adel al-Hemiri and Wasan O. Noori

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IJCPE Vol.10 No.1 (March 2009)

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