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Extraction

Removal of soluble material from insoluble residue,


either solid or liquid, by treatment with a liquid solvent.
➢ It is a solution process and depends on mass transfer
phenomena (solute diffusion to the bulk solution).
➢ Solutes are separated based on their different
solubility's in different liquid
➢ The controlling factor in the rate of extraction is
normally the rate of diffusion of the solute through
the liquid boundary layer or layers at the interface.
Methods of extraction :

1. Infusion
2. Decoction
3. Digestion
4. Maceration
5. Percolation
1. Infusion

Fresh infusions are prepared by macerating


the crude drug for a short time with cold or
boiling water. These are dilute solutions of
the readily soluble constituents of crude
drugs.
Types of Infusion
Fresh Infusion : e.g. Infusion of orange
Concentrated Infusion : e.g. Concentrated infusion of
medicinal plants
2. Decoction :

In this process, the crude drug is


boiled in a specified volume of
water for a defined time; it is then
cooled and filtered. This procedure
is suitable for extracting water-
soluble, heat stable constituents.
e.g. Tea , Coffee
3. Digestion :
➢ T his is a form of maceration in which gentle
heat is used during the process of extraction.
➢ I t is used when moderately
elevated temperature is not objectionable.
e.g. Extraction of Morphine
4. 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 decantation, after standing.
5. 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 preparation of tinctures and fluid extracts.
➢ It is the method of short successive maceration or
process of displacement
➢ A percolator (a narrow, cone-shaped vessel open at
both ends) is generally used.
Steps in percolation
1. Size reduction: The drug to be extracted is subjected
to suitable degree of size reduction,
2. Imbibition: During imbibition the powdered drug is
moistened with a suitable amount of
solvent for 4 hrs in a well closed container.
3. Packing: After imbibition the moistened drug is evenly
packed into the percolator.
4. Maceration: After packing sufficient solvent is added to
saturate the material. The percolator is allowed to stand
for 24 hours to macerate the drug.
5. Percolation: The lower tap is opened and liquid
collected therein is allowed to drip slowly at a controlled
rate.
Processes of Extraction:

1. Solid / liquid extraction

2. Liquid / liquid extraction


1. Solid-liquid extraction
Extraction of soluble constituent from a solid by means of
a solvent is referred to as "leaching" or "extraction".
➢ This process is an important stage in the production of
many natural chemicals found in animal or vegetable
tissues.
Example:
1. Extraction of fixed oils from seeds.
This offers an alternative method to mechanical expression
2. The preparation of alkaloids such as strychnine from
Nux Vomica beans or quinine from Cinchona bark
3. The isolation of enzymes such as Renin
4. Hormones such as insulin from animal source.
There are two ways of leaching:
1. Leaching by percolation
a. Stationary-bed leaching (batch operation)
b. Moving-bed leaching (continuous operation)

Percolate = Solvent be passed through bed


[Stationary-bed - Moving-bed ]

2. Leaching by immersion
Factors influencing rate of leaching

The controlling factor in the rate of extraction is


normally the rate of diffusion
Any factor that enhances diffusion ⇒ enhancement of
leaching
Factors influencing rate of leaching
1. Particle size
2. Solvent used
3. Temperature
4. Agitation of the fluid
1. Particle Size

⇊ of solid particle size ⇨ ⇈ surface area available for


extraction ⇨ ⇊ the distance which the solute covers
from the inside of particles to outside.
Reduction of particle size should be controlled since very
fine particle may:
1. Inhibit the solvent circulation (cause blokage).
2. Increase electrostatic charges on the surface of the
particles, which adsorb the extracted solute on their
surfaces and decrease the efficiency of extraction.
3. Less selective extraction.
2. Temperature

The ⇧ temperature: ⇒⇈ the solubility of most


solutes ⇒ ⇊ the viscosity of solvent and facilitates
its diffusion to the solid to be extracted.
But also temperature should be controlled to
avoid:
1. Inhibition of enzymatic activity.
2. Decomposition of active constituents.
3. Solvent

Should be selective for the solute, cheap, non-


toxic, stable and non-inflammable
N.B. as the extraction process proceeds ⇒
the concentration gradient ⇊ (between the
solvent and solid substances) and also ⇈ solvent
viscosity ⇒hindering the extraction process.
4. Agitation of the fluid

Agitation facilitates diffusion of solute to the


bulk of solution.
Agitation keeps fine particles in suspension
and facilitates solvent penetration.
Leaching By Percolation

1. Stationary-bed leaching
(batch operation)

It is suitable for preparation of concentrated


alkaloidal extracts by percolation.
Batch Percolator
➢ It is composed of a tank with a
perforated false bottom to
support the solids and permit
drainage of the solvent.
➢ The solids are loaded into the
tank, sprayed with solvent until
their solute content is reduced to
economical minimum (i.e.,
exhausted).
Batch Percolator
➢ The body of extractor may be
jacketed to give control of
the temperature.
➢ Extraction is stopped when
leach liquid is free from
constituents.
Requirements of operation:
➢ Large amount of solvent is needed to deplete drug
from solid, thus the yield extract is diluted.
To overcome such disadvantage:
➢ the extraction is followed by evaporation.
➢ evaporation under reduced pressure → heat
sensitive material.
➢ Vapor leaving the evaporator is condensed and
returned to extractor
Leaching By Percolation

2. Continuous Moving
Bed Leaching
(Bollman Extractor)
Bellman Extractor

• Vertical chamber in
which baskets with
perforated metal
bottoms are carried on
a chain running over
two wheels.
Bollman Extractor

➢ Baskets then come under


feed hopper and filled with
fresh seed.
➢ As they descend, they are
spayed with the half
miscella near top of column,
which then percolates down
through the baskets in the
descending column and
collects in bottom, as fully
concentrated miscella.
Bollman Extractor

➢ As the basket rises, fresh


solvent is added into each
basket as it reaches the top
of the column, so that the
solvent with oil it contains
percolates down through the
seeds in the rest of the
basket in the rising column.
Bollman Extractor

➢ The resulting dilute solution


collects in the bottom of the
apparatus. It is called half
miscella (solution of oil /
solvent)
➢ At top of the travel, the baskets
are inverted, the exhaust is
discharged into chute, from
which it is removed by a screw
conveyor.
B. Liquid-liquid
extraction
EXTRACTION TOWERS
Principles
two immiscible solvents brought into intimate contact
to allow transfer of drug from one to another (in which it
is more soluble),
Two immiscible liquid phases flowing counter-current to
each other.
Heavy phase is introduced at the top while lighter phase
is introduced at the bottom.
All extraction equipment use a gravitational force to
effect counter-current motion and separation of the two
phases due to density differences.
successful liquid–liquid extraction depends
upon efficient dispersion of one phase into
another to maximize the contact area
between phases, whilst also enabling phases
to be subsequently separated without the
formation of a stable emulsion.
Application
1. Refining of vegetable oils
2. Applied in the manufacture of pharmaceuticals
such as antibiotics
Classification

1. plate column (ex. Baffle plate column)


2. Spray column
Baffle Plate Column
➢ They are simple cylindrical columns
provided with alternate horizontal
baffles to direct the flow of the
dispersed phase in zigzag path. 75%
diameter
➢ Heavy liquid flows over the top of
each baffle and cascades to the
one beneath; light liquid flows
under each baffle and sprays
upward from the edge through the
heavy phase.
➢ Contact be tween liquids occur
at edge of plates
2. Spray Columns:
➢ Simple extraction towers
➢ Empty towers without packing
or baffles
➢ One liquid fills the whole
tower (continuous phase),
while the other phase is
dispersed through it by
spraying
➢ N.B: Towers are very long constructions.

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