EXTRACTION AND

SEPARATION TECHNIQUES
 Extraction
 Extraction is the method of removing active constituents from a
solid or liquid by means of liquid solvent.
 The separation of medicinally active portions of plant or animal
tissues from the inactive or inert components by using selective
solvents.
 In this method the wanted components are dissolved by the use of
selective solvents known as menstrum & undissolved part is a marc.
After the extraction unwanted matter is removed.
Extracts are prepared by using ethanol or other suitable solvent.
Extract : Extracts can be defined as preparations of components
which contain all the constituents which are soluble in the solvent.

Marc: Solid residue obtain after

extraction
Menstruum: Solvent used for extraction
• Dissolution of extractive substances out of
disintegrated cells.

• Dissolution of extractive substances out of

intact plant cell by diffusion (requires
steeping and swelling)

• Penetration of the solvent into the plant cells

and swelling of the cells.

• Diffusion of the dissolved extractive

substances out of the cell.
•Plant constituents are usually contained inside the cells.
Therefore, solvent used for extraction must diffuse into
the cell to dissolve the desired compounds where upon
the solution must pass the cell wall in the opposite
direction and mix with the surrounding liquid.

•An equilibrium is established between the solute

inside the cells the solvent surrounding the
and
fragmented plant tissues
 Ideal properties of the solvents :

• Be highly selective for the compound to be extracted.

• Not react with the extracted compound or with other compounds in the plant material
• Have a low price.
• Be harmless to man and to the environment.
• Be completely volatile.
• Should not mix up with water.
• Should have the big capacity in relation to extractive.

• The density of solvent should be difference from water density.

• Should have the minimum viscosity.
 Mechanism of Extraction

solvent 2

Plant cell

1
3
Factors affecting extraction process

•Nature of compound
•Solvent
•Temperature
•pH
•Particle size

8
 Methods of extraction
Infusion
Decoction
Digestion
Maceratio
n
Percolatio
n
Continues
hot
extraction
Supercritical fluid extraction
Counter current extraction
Microwave assisted extraction
 Infusion :
Fresh infusions are prepared by
macerating the crude compounds
for a short period of time with cold
or boiling water. These are dilute
solutions of the readily
soluble constituents of crude
compounds.
Types of Infusion :
Fresh Infusion: e.g. Infusion of orange
Concentrated Infusion : e.g. Concentrated
infusion of Quassia
Decoction :
In this process, the crude
drug is boiled in a specified
volume of water for a
defined time; it is then
cooled and strained or
filtered. This procedure is
suitable for extracting water-
soluble,
heat stable constituents.
e.g. Tea , Coffee
 Digestion
:

This is a form of maceration where gentle

heat is used during the process of
extraction.

It is used when moderately elevated

temperature is not objectionable.

The solvent efficiency of the menstruum is

thereby increased.

e.g. Extraction of Morphine

 Maceration
:
In this process solid ingredients
are placed in a stoppered
container with the whole of the
solvent and allowed to stand for a
period of at
least 3 days (3 - 7 days) with frequent
agitation, until soluble matter is
dissolved.

The mixture is then strained (through

sieves/nets), the marc pressed and the
combined liquids clarified
(cleaned by filtration) or by
 Process of maceration :
Plant Material
(Crushed or cut small or Placed in a closed vessels
Moderately coarse
powder)

Allowed to stand for seven Whole of the selected

days shaking occasionally solvent (Menstruum)added

Solid residue (marc)

Liquid strained off pressed(Recover as much
as occluded solution)

Clarified by subsidence (Strained and

or filtration expressed liquids
mixed)

Evaporation and Concentration

 Types of maceration :
•Simple maceration: for organized and unorganized Crude
drug
e.g. i) Tincture of Orange
ii) Tincture of Lemon
iii) Tincture of Squill
• Double maceration :
Concentrated infusion of
orange
• Triple maceration: The maceration process may
be carried out with help of heat or stirring
e.g. i) Concentrated infusion of Quassia
ii) Concentrated infusion of Senna
 Factors affecting Maceration
Concentration gradient (C1-C2) is affected by several factors
1. Solid/solvent ratio: Yield decreases with constant quantity of solvent and
increasing proportion of drug material.
2. Dissolution from disintegrated cells: Particle size
3. Steeping and swelling of plant material: Capillary dilation and increase in
diffusion rate (Mucilage)
4. Diffusion from intact plant cell: Solvent must be able to solublilize
substances
5. Temperature: increase solubility (diffusion coefficient), and decrease the
viscosity
6. pH value: Influence the selectivity of extraction (qualitative and
quantitative)
[Link] of dissolved constituents with insoluble support material of plant
[Link] of lipophilicity

[Link] of addition of surfactants, salts and co-solvents

 Merits
•Small sample size.
•Strong swelling properties or high
mucilage.
•Energy saving process.

Demerits
•N o t exhaustively extract thedrug.
•I t is very slow process.
•Solvent required is more.
 Percolation
It is continuous downward displacement of
the solvent through the bed of crude
drug material to get extract.

Most frequently used to extract

active ingredients in the
separation of soluble compounds .

It is the method of short successive

maceration or process of displacement

A percolator (a narrow, cone-shaped

vessel open at both ends) is conical cylindrical
generally used.
24
 Steps in percolation
[Link] reduction: The drug to be extracted is subjected to suitable
degree of size reduction, usually from coarse powder to fine
powder.
[Link]: During imbibition the powdered drug is moistened
with a suitable amount of menstruum and allowed to stand for
four hours in a well closed container.
3. Packing: After imbibition the moistened drug is evenly packed
into the percolator.
[Link]: After packing sufficient menstruum is added to
saturate the material. The percolator is allowed to stand for 24
hours to macerate the drug.
[Link]: The lower tap is opened and liquid collected therein
is allowed to drip slowly at a controlled rate until 3/4th volume of
the finished product is obtained.
 Types of Percolation
[Link] Percolation :
Percolation and
Sample Imbibition Maceration collect the percolate
For 4 For 24 hours i.e.3/4th of the volume
hours of finished
e.g. i) Tincture of Belladonna preparation
ii) Compound tincture of
cardamom
2. Modified Percolation :
-Repeated maceration is more effective than simple.
-Multiple maceration – Solvent divided into equal multiple
time considering the solvent retained by plant tissue.
-Used to prepare concentrated preparation.
Merits :
•Requires less time than maceration.
•Extraction of thermolabile constituents can be possible.

Demerits :
•Requires more time than soxhalation.
•More solvent is required.
•Skilled person is required.
 Maceration Vs Percolation

 Maceration  Percolation
Time consuming and also
extraction is not complete
 short time and more complete
extraction
Not required skilled operator
 Skilled operator is required
For certain substances which are
very less soluble in solvent and Special attention should be paid
requires only prolonged contact on particle size of material and
with solvent. throughout process.
Suitable method for less potent
and cheap drugs  Suitable method for potent and
costly drugs

29
Soxhalation

Condenser

Side
tube
Syphon Thimble
tube

Distillation flask

Heating Mantle
THE SOXHLET EXTRACTOR: Continuous extraction of a
component from a solid mixture.

Boiling solvent vapors rise up through the larger side arm.

Condensed drops of solvent fall into the porous cup,
dissolving out the desired component from a solid mixture.

When the smaller side-arm fills to overflowing, it initiates a

siphoning action.

The solvent, containing the dissolved component, is

siphoned into the boiler below residual solvent then drains
out of the porous cup, as fresh solvent drops continue to
fall into the porous cup and the cycle repeats .
Merits
• Large amount of drug can be extracted with much smaller
quantity of solvent.
• Tremendous economy in terms of time, energy & ultimately
financial inputs.
•Small scale used a batch-process.
•Becomes more economical when converted into continuous
extraction.
•Procedure on large scale.
Demerits
•Physical nature of drug.
Solvent.
•Chemical constituent of drug.
 Supercritical Fluid Extraction
F o r every substance, there is a critical temperature (Tc) and
pressure (Pc) above which no applied pressure can force the
substance into its liquid phase. If the temperature and pressure
of a substance are both higher than the Tc and Pc for that
substance, the substance is defined as a supercritical fluid.
 Properties of SCFs
At the critical point, the density of the gas and liquid
phases is the same; there is no distinction between
the phases. i.e. between those of the pure liquid and
gas.

Supercritical posses densities that are liquid-like

and Transport properties that are gas-like.

These offersgood penetrative ability and good

extractive ability.
 Choice of SCFs
solvent
- Good solving property
- Inert to the product
- Easy separation from the product
-Cheap
- L o w CP because of
economicreasons SCF, due
-Carbon
primarilydioxide is critical
to its low the most parameters
used (31.1°C, 73.8
bar)
-non-toxicity.
However, several other SCFs have been used in both
commercial and development processes. The critical
properties of some commonly used SCFs are -
Fluid Critical Critical Pressure
Temperature (K) (bar)

Carbon dioxide 304.1 73.8

Ethane 305.4 48.8

Ethylene 282.4 50.4

Propane 369.8 42.5

Propylene 364.9 46.0

Trifluoromethan
299.3 48.6
e
(Fluoroform)
Chlorotrifluoromethane 302.0 38.7
 Supercritical Fluid Extraction Process :
 The oldest typical and
most common supercritical
fluid extraction from solids is
performed as a batch process,
with a continuous flow of SCF.

 An extraction medium
(going to be SCF) stored in
the feed tank and liquid SCF
is pumped from a
reservoir ;
it is heated and pressurized to
reach the supercritical conditions.
 Supercritical Fluid Extraction
 extraction chamber where
contact with crude drug bed
occurs and the more volatile
substances are dissolved
into the supercritical fluid.
Solute and SCF leave
extractor and extract is
precipitated in
separators, where SCF
becomes gaseous.
Gas is recycled by
condensation before
returning to liquid
reservoir.
 Advantages
• Dissolving power of the SCF is controlled by pressure and/or
temperature.

• SCF is easily recoverable from the extract due to its volatility.

• Non-toxic solvents leave no harmful residue.

• High boiling components are extracted at relatively low temperatures.

• Separations not possible by more traditional processes can sometimes be

effected.

• Thermally labile compounds can be extracted with minimal damage as

low temperatures can be employed by the extraction.
 Disadvantages

 Elevated pressure required.

 Compression of solvent requires elaborate recycling measures
to reduce energy costs.
 High capital investment for equipment.
 Applications
• Recovery of organics from oil shale
• Separations of biological fluids
• Bioseparation
• Petroleum recovery
• Crude dewaxing
• Coal processing (reactive extraction and liquefaction)
• Selective extraction of fragrances, oils and impurities
from agricultural and food products
• Pollution control
• Combustion and many other applications.
 Counter-Current Extraction
 A liquid-liquid extraction process in which the solvent and
the process stream in contact with each other flow in
opposite
directions.

 Screw extractors andcarousel extractors are the two

type of equipments used for Counter-Current Extraction.
 Counter-Current Extraction Process
• In counter-current extraction (CCE), wet raw material is
pulverized using toothed disc disintegrators to produce
fine slurry.

• The material to be extracted is moved in one direction

(generally in the form of fine slurry) within a cylindrical
extractor where it comes in contact with extraction
solvent.

• The further the starting material moves, the

more concentrated the extract becomes.

• Finally, sufficiently concentrated extract comes out at one

end of the extractor while the marc (practically free of visible
solvent) falls out from the other end.
 Advantages
1. A unit quantity of the plant material can be extracted with much
smaller volume of solvent as compared to other methods like
maceration, decoction, and percolation.
2. CCE is commonly done at room temperature, which
spares the thermolabile constituents from exposure to
heat which is employed in most other
techniques.
3. As the pulverization of the drug is done under wet
conditions, the heat generated during comminution is
neutralized by water. This again spares the
thermolabile constituents from exposure to heat.
4. The extraction procedure has been rated to be
more efficient and effective than
Continuous hot extraction.
 Applications :

1. DNA purification.

2. Food Industry.

eg. Citrus oils, Unsaturated fatty acids, and

tocopherol.
squalene
3. An important application is citrus oil processing,
An important subject in perfumes and food industries.