Extraction methods
5th sem Bpharm
Extraction
• Extraction is the process in which the separation of the
soluble constituents occurs from insoluble substance
either solid or liquid by processing with a specific solvent.
• Factors which effect the process of mass transfer are
temperature, agitation, size reduction and others.
• Menstrum: Solvent or mixture of solvent use for extraction.
• Miscella: Solution with extracted substance.
• Marc: Residue left after extracting the desired constituents.
The various methods of extraction are:
1. Infusion [Link] continuous extraction
(soxhalation)
2. Decoction
8. Percolation
3. Digestion
9. Ultra sound extraction
4. Maceration
[Link] current
10. Steam distillation
extraction
11. Microwave assisted extraction
6. Super critical fluid
extraction
INFUSION
• In the infusion process the crude drug is left with solvent to
soak them properly at room temperature for a particular
period of time with or without intermittent shaking.
• The infusion process is generally followed when active
constituents are water soluble and they are soft in nature so
that water can penetrate into the tissue.
• The final volume is not adjusted in infusion. Infusion can be
fresh or concentrated. Examples are Infusion of quassia,
senna.
DECOCTION
• The process is more suitable for the vegetables drugs
which are heat stable and water soluble because in this
method the drug is boiled for about 15 min.
Take drug in a vessel add 1000 ml water and cover it
Boil this for around 15 minutes
Cool it to room temperature
Strain the liquids and press the marc
– Herbal tea and coffee is good example of
decoction.
DIGESTION
• Digestion is modified form of maceration in which the
temperature of the menstrum is kept heated at particular
temperature at under pressure.
• This rise of temperature and pressure help the menstrum to
penetrate the drug and extract it completely.
• The apparatus use for the digestion is the digestor which is
generally made up of metal.
MACERATION
• In the process of maceration the crude drug is immersed into the
bulk of menstrum or solvent for at least 3 days (generally 3-7 days).
• During this period the menstrum is agitated frequently.
• The menstrum and the drug should be kept in the stoppered
container to avoid the loss of solvent by evaporation.
• The mixture is then filtered or strained through net or sieves and
then press the marc and clarify liquid by decantation after standing.
• Frequent agitation help the distribution of active constituents in the
entire solvent and prevent localization of active constituents around
the tissue and cell.
Maceration may be of various types like:
1. Simple
2. Modified
3. Multiple
4. Kinetic maceration
5. Remaceration
Uses of Maceration:
BP permits the preparation of the tincture by maceration
methods of following drugs
• Squill tincture, Catechu tinctures, Senna liquid extract
compound Benzoin tincture and opium tincture.
• Mother tinctures of homeopathic Pharmacopoeia are
prepared by maceration methods.
• Maceration is most widely used method of extraction.
PERCOLATION
• Percolation can be defined as 'Short successive
maceration or extraction by the method of
displacement'.
• Percolation can be performed into the conical percolator,
cylindrical percolator or steam jacketed percolator.
• The various stages involved in the percolation are
following:
(a)Size reduction
(b) Imbibition
(c) Packing:
(d) Maceration:
(e) Percolation
(f) Pressing the marc
(a)Size reduction
• To assure the complete exhaustion of the crude drug,
the drug should be suitably size reduced.
• Size reduction helps in
– increasing the surface area of the crude drug
– uniform packing of crude drug in percolator and
reduce the amount of menstrum in the percolator.
(b) Imbibition:
• Imbibition is a process in which the powdered drug is
kept along with menstrum for 4 hours in a well
stoppered container. During this duration the
menstrum penetrate into cell wall.
(c) Packing: The packing should be perfect, neither too tight
nor too loose which may affect the flow of menstrum.
• Two third of the percolator should be cover with the drug
on which place the piece of filter paper and wash sand
should be placed on the top of the filter paper.
(d) Maceration : Sufficient amount of menstrum should be
added after packing and allowed to stand, the percolator
for 24 hours as the primarily maceration take place.
(e) Percolation: After 24 hours of maceration, collect the
menstrum from lower end until the three fourth portion of
the final product is obtained.
Completion of the percolation process should be check by
various method like:
By checking the specific gravity of end few ml of percolate and
compare with the specific gravity of fresh menstrum.
Evaporate the last few ml of percolate to dryness and see that
any residue comes after evaporation or not.
Perform the specific chemical test for last few ml of percolate
like tannins, glycoside, alkaloids etc whether it is positive or
negative.
(f) Pressing the marc: In the last, the marc should be pressed and
obtain liquid is added into the collected menstrum. More
menstrum should be added to obtain the desired volume.
• Example-Strong tincture of ginger, tincture of belladona etc.
Modifications :
• Modified Percolation
• Intermittent percolation
• Re-percolation
• Hot percolation
• Reserved percolation
• Circulatory percolation
• Diffusion percolation
Soxhlet Extraction/Continuous Hot Percolation
Process:
This extraction process is more suitable where menstrum have less
penetration into the cellular tissue.
Active constituent are not readily extracted with solvent.
The quantity of solvent for extraction of the active constituents is
very less.
The hot menstrum is passed again and again over the crude drug
and solubilize its active ingredient until the drug become exhausted.
The apparatus consist of three important parts:
(a) A round bottom flask (RBF) which contain menstrum.
(b) Extraction chamber in which drug is kept in thimble.
(c) Condenser.
Firstly, the size reduced drug is packed into the thimble (made of
filter paper or cellulose) which is helpful to prevent choking of the
extractor.
Place the solvent in the round bottom flask (RBF) and boiled it by
heating mantle. The vapour of the solvent goes to the condenser
via side tube.
Condenser condenses the vapour of solvent and this solvent
penetrates the packed drug. It percolates the crude drug and
extracted the active ingredient.
The level of menstrum is increased in the extractor until it reaches
to maximum point from where it is siphoned into the round bottom
flask.
This menstrum is again heated in RBF where active constituent
remain in RBF and vaporized solvent again pass through the side
tube and condenser, which penetrates the drug present in the
extractor.
The process will continue till the drug become exhausted.
Disadvantages
• Thermolabile drugs and constituents are not suitably extracted by
this method because the active ingredient may be destroyed.
• Pure solvent or only those solvent mixtures which have constant
boiling temperature can be used for extraction purpose.
• Some drug like resin, opium, gum etc blocks the Soxhlet apparatus
so this is not suitable method for these drugs.
MICROWAVE ASSISTED EXTRACTION
• The electromagnetic radiation which have a frequency 0.3-300 GHz
are called microwave.
• Industrial microwaves are generally operated at 2.45 GHz so that it
can avoid the interferences of domestic instruments like radio and
other.
• Due to their electromagnetic property microwaves contain
magnetic and electric field. They are perpendicular to one another.
• Electric field generates heat through two simultaneous method i.e.
ionic conduction and dipolar rotation.
• Microwave transfer the energy to solid matrix and solvent
homogenously and very efficiently.
• Substance absorb the energy as per dielectric constant ; which
causes the heating of moisture present inside the drug.
• Evaporation occurs due to heating of moisture and this will
produce high vapour pressure- results in cracking the cell wall
of plant drug and release the active constituent into the
solvent.
• The extraction property of the solvent and their interaction
with microwave can be altered by using solvent mixtures.
Advantages
• less solvent are required, time consumption is less, high
extraction rate and good reproducibility
Disadvantages
• Additional centrifugation or filtration are necessary to remove
residue and the efficiency will be poor if the solvent or
compound have non polar property or they are volatile.
Example- Extract of glycyrrhizic acid
ULTRASONIC ASSISTED EXTRACTION
• The frequencies above the 20,000 Hz known as ultrasound
are used in ultrasonic extraction.
• These waves cause cavitations effect on the dry cell and
destruct the cell wall and release the active constituents.
• When ultrasonic waves are passed through the liquid media it
compresses (produce high pressure) and rarefaction (low
pressure) to the liquid media.
• Due to this process small voids or vacuum bubbles are formed
in the solvent.
• After certain duration these bubbles are not able to absorb more
energy produce by microwave and they burst.
• At the high pressure cycle they bursts, which is known as
cavitation. Due to this cavitation, cell wall destructed and active
chemical constituent are extracted.
Advantage
• This process is efficient, inexpensive and simple compare to
conventional extraction techniques.
• It has high yield, reduce operating temperature and easy to
operate
Disadvantage
• Sometime active constituent can convert into free radical which
have undesirable side effect.
STEAM DISTILLATION
• It is one of the most popular methods to separate the
essential oil from the crude drugs.
• A still (large stainless steel container) contain the crude drug
material. The steam is injected through inlet valve into the
plant material which contains the essential oil.
• The inlet steam evaporates the volatile molecule which is
collected into the condenser.
• The water molecule and volatile oil molecule can be easily
separated because they are not mixable.
• Direct prolonged heating should be avoided which
deteriorates the volatile components.
COUNTER CURRENT EXTRACTION
• In counter current extraction the substance which is to be
extracted is distributed between two different solvent depends
upon their distribution coefficient.
• This can be best performed by Craig apparatus. There are number
of glass tubes (r = 0, 1, 2, 3, ----) in the Craig apparatus
• They are designed such that the solvent which are lighter in density
can be transferred from first tube to second tube and then forward.
• The tubes are driven or shaken electromechanically. The lower
phase which have higher density is called as stationary phase and
the solvent which have the lighter density is called the mobile
phase.
• The substance to be extracted is present in the stationary
phase. Equal quantity of stationary phase is present in all
the tubes.
• The mobile phase is transferred into the first tube (tube
=0) shake properly so that extraction take place and then
phases are allowed to separate down.
• The mobile phase then transferred to next tube no 1 and
repeat the same process and transfer it into further tube
like tube no 2, 3, 4 and so on.
• The substance having higher distribution ratio separate
more quickly compare to lower distribution ratio.
• Craig apparatus is now less frequently used because of
the availability of more recent chromatographic
techniques.
• It is very difficult to construct and operate a Craig
apparatus having more than 100 test tubes.
SUPER CRITICAL FLUID EXTRACTION
• A critical point is a particular temperature and pressure at
which two phases (like liquid and vapour) can co-exist.
• The substance at above the critical temperature and pressure
or above the critical point is known as supercritical fluid.
• The property of super critical fluid is in between gas and pure
liquid so that they are also known as dense gases or
compressible liquid.
• Super critical fluid has good solvation power, low viscosity,
higher diffusibility and good penetrating power.
• By this method, we can separate the constituents from
the solid matrix but it may also be liquid.
• CO2 is one of the most common super critical fluid.
• To make CO2 super critical fluid the critical
temperature is 31°C and critical pressure is 74 bars.
Instrumentation:
• There are different components in the super critical
fluid extraction apparatus. First one is fluid reservoir
which contains the fluid like gas cylinder in the case of
CO2.
• Another one is the pump; the pump may be syringe
pump or reciprocating pump.
• Another important is the extractor which may be made
of stainless steel and can with stand to high pressure
like 300 to 600 atmosphere.
• Another important component of the super critical fluid extractor is
the restrictor. It is important for the controlled and systematic
release of the pressure inside the extractor vesicle. The restrictor
may be fixed type or variable type.
• The isolated constituent is collected in a collector where it can be
detected with the help of detector.
• Sometimes modifiers are also added into the supercritical fluid to
increase its versatility like one to ten percent of methanol is added
in CO2.
• During the process the liquid is pumped into a
heating zone and heated to supercritical
temperature then the super critical fluid passes
through the extraction vessel where it diffuses to
the solid matrix and dissolves the active
constituents.
• The extracted material with super critical fluid
comes into the separator or collector unit where
the pressure is low.
• The extracted material settle down here and the
CO2 can then be cooled, recycled or discharge to
the environment. The isolated constituent can be
detected with the help of detector.
Advantages and Limitations:
• The super critical fluid extraction technique is very rapid
and there is no need of organic solvent for the extraction
purpose. The thermolabile substance can also be
extracted with this technique. It is a versatile and
efficient continuous method with complete separation
and recovery of the solvent.
• Sometimes its consistency and reproducibility may vary.
It is expensive technique because it need high pressure
which increases its cost.
• CO2 cannot always be used as solvent as it is non polar
and so limited dissolving power particularly in case of
polar solvent.