Percolation FA19 PHM-3

PERCOLATION
Derived from the Latin word “per” and “colare”which means “through strains”.
Percolation can be defined as

“The process of extracting the soluble constituents of a powdered drug by the passage of
liquid through it”.

STEPS OF PERCOLATION
1. Size reduction or comminution of the drug
2. Pre-treatment (Imbibitions)
3. Packaging
4. Maceration
5. Percolation
6. Volume adjustment

Size reduction
The drug to be extracted is subjected to suitable degree of size reduction, usually
from coarse powder to fine powder,
1. To increase the surface area of drug,
2. For uniform packing of the percolator,
3. To slow down the movement of menstrum,
4. To ensure complete exhaustion of drug.

Imbibition
During imbibition the powder drug is moistened with the suitable amount of solvent and
allowed to stand for four hours in a well-closed container. During this period the drug
swells up and menstrum penetrates the cell walls. After the lapse of time, the moistened
drug is passed through a coarse sieve to remove the lumps and to mix the dry powder, if
any.
This preliminary moistening of drug is necessary because of the following reasons
1. The dried tissue swells when it comes in contact with menstrum. If the drug is packed
in the dry condition, subsequent swelling will reduce the porosity of the material and
choke the percolator. This swelling is particularly important with the aquous solutions
2. The air between the interstices is removed by menstrum, which will otherwise disturb
the packing of the percolator due to which the menstrum will run mainly through the
channel resulting in inefficient extraction.
3. preliminary moistening also makes the fine particles less liable to wash out of the
column during percolaton

Packing
After imbibition the moistened drug is evenly packed into a percolator.
A percolator may have following parts.
1. A percolator is conical vessel or a cylinder having a lid at the top
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2. The percolator is provided with a false bottom that is a perforated plate on which
filter paper or cotton wool is placed to support the column of the drug and help in
the escape of the percolate.
3. The base of the percolator is fitted with a tap from which the percolate is
collected.
4. A pipe may be connected to the tap to lead the percolate away for further
processes or to an other percolator to use the menstrum more efficiently.

On a small scale glass percolators are used and the raw material is placed on a loose plug
of cotton that has been moistened with water previously.

Two types of percolator are available

 Open percolator
 Close percolator
Open percolator:
Open percolator is cheap and easy to handle. it is used when the menstrum is water or
dilute alcohol.
Close percolator:
Close percolator is used when the menstrum is volatile e.g. alcohol, ether etc. if the
percolation is to be carried out at elevated temperature then steam jacketed percolator
may be used.

For packing, a piece of cotton wool, fibers of flax, hemp or any other suitable material;
previously moistened with menstrum is placed on the false bottom of the percolator. A
small amount of the moistened drug is introduced into the percolator and is pressed
lightly with rod or any other suitable device, to give even compression, similarly, more of
the moistened drug is introduced and pressed till whole of the drug is packed into the
percolator. The packing should not be too tight, it will not allow the menstrum to pass
freely which will lead to slow extraction rate. Similarly loose packing will allow
menstrum to pass through quickly resulting in complete contact with the drug, hence less
dissolution of active constituents.

Precaution
should be taken that the drug should occupy 2/3 rd capacity of the percolator. After
suitable packing of the drug into the percolator a piece of filter paper is placed over top
of it on which small quantity of washed sand is placed to prevent disturbance of the
packed material.

Maceration
After packing the column, sufficient menstrum is added to saturate the material and top
of the percolator is covered with a lid. When the liquid begins to drip from the bottom of
the percolator, the tap fitted at its bottom is closed, if need arises then more of menstrum
over the drug. Under no circumstances the column should be allowed to become dry
otherwise cracks will appear in the packed column resulting in inefficient percolator. The
percolator is then set aside for 24 hours to macerate the drug. This period helps the
 Percolation FA19 PHM-3

menstrum to percolate deep into the tissues and dissolve the maximum amount of active
constituents and drug will be extracted with comparatively small volume of menstrum

Percolation
After 24 hours maceration of the drug the lower tap of the percolator is opened and the
liquid collected there in is allowed to drip slowly at a controlled speed until 3/4 th vol. of
the finished product is obtained.
Sufficient menstrum is simultaneously added over the drug because at on time packed
material should be allowed to become dry.
To avoid adding the menstrum time and again, a bottle full of menstrum carrying the
delivery tube to the percolator may be fitted in the inverted position which will supply the
menstrum continuously over the top of the percolator.
After collecting 3/4th vol. the percolate is tested for complete exhaustion of the drug by
various test,

The marc is then pressed and expressed liquid is added to the already collected percolator
which should be about 80-90% of the final vol. More of menstrum is added to produce
the required vol.
The liquid is then allowed to stand to settle the suspended partiales,decanted or clarified
by filtration.

Test for checking complete exhaustion of drug

 Take a few ml of the last percolate and evaporate to dryness, if no residue remains
this shows that the drug is completely exhausted.
 Measure the specific gravity of the last few ml of percolate if it is equal to the specific
gravity of the menstrum, it shows exhaustion of drug.
 Specific test may be performed on the percolate for the drug containing alkaloids ,
glycosides , tannins , resins or bitter constituents.

Volume adjustment
In some cases additional ingredients e.g. glycols are added before final adjustment.
In the case of more potent tinctures the percolate is assayed and calculated amount of
menstrum is required to give a product of required strength is added.
The marc is expressed after the exhaustion of drug, objective is to avoid the wastage of
the menstrum.
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RESERVED PERCOLATION
Percolation process in which first portion of the percolate is reserved which contain the
max. Amount of active constituents.
Subsequent percolation is completed as usual .
The last part is collected separated .
The second dilute part is then evaporated to get a syrupy consistency which is then mixed
with the reserved portion of the percolate
The final volume is adjusted by adding more of menstrum.
Alcohol is used as menstrum in this process.

Advantages
The reserved part of percolate which contain the maximum amount of dissolved principle
is not subjected to heat treatment for evaporation, only the dilute portion of percolate is
evaporated .

This process is economical as whole of the percolate is not evaporated .

CONTINUOUS HOT PERCOLATION PROCESS OR SOXHLET EXTRACTION

Continuous hot percolation process is used for those drugs where the penetration of
menstrum into the cellular tissues is very slow and the solute is not readily soluble into
the solvent and the quantity of menstrum is very less.
In such cases soxhlet extractor is used where small vol. of hot menstrum is passed over
the drug time and again to dissolve out the active constituents until the drug is exhausted.
This process is known as SOXHLATION

The soxhlet apparatus required for the continuous hot percolation is made from a very
high grade of glass and consist of three parts
A flask in which the menstrum is boiled
An extraction chamber in which drug is fitted,
is fitted with a side tube and a siphon
A condenser

The drug to be extracted ,in suitable comminuted form is usually packed in a “thimble”
made of filter paper which is then placed into the wider part of the extractor
Thimble is used to prevent choking of the lower part of the extractor by drug particles.
Menstrum is placed in the flask and boiled, the vapors are allowed to pass through the
side tube to the condenser where they are condensed and fall on to the packed drug,
through which it percolates and extract out the active constituents.
As the vol. of menstrum in the extractor increases, the level of liquid in the siphon also
increases till it reaches the max. point from where it is siphoned out in the flask.
On further heating,the menstrum vaporizes while the dissolved active constituents remain
behind in the flask
The alternate filling and emptying of the body of the extractor goes on continuously till
the drug is exhausted.
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The the same quantity of menstrum is made to percolate repeatedly, about 14 to 15 times
through the drug and the active constituents are collected in the flask.
DISADVANTAGES

This process is not suitable for the drug containing thermolabile active constituents.