Different methods of extraction

• Phytochemicals are naturally occurring chemical

compounds in plant-based foods.

• Phytochemistry is concerned with the enormous

variety of organic substances that are elaborated
and accumulated by plants and deals with the
chemical structures of those substances, their
natural distribution and their biological function.

• In all these operations, methods are needed for

separation, purification, extraction of many
different constituents present in plants.
Extraction
The process of separating active principle(s)
from powdered crude drugs by using suitable
solvents is called extraction.

• Removal of soluble material from the insoluble

residue, either liquid or solid, by treatment with a
liquid solvent.
• The solvent used for extraction is called menstruum
& the undissolved residue left behind is called marc.
• The extracted preparation is known as Galenicals.
Factors affecting on extraction of drugs:
• Character of drug: Hard or soft drugs.
• Stability of drug: Thermolabile or
thermostatic.
• Concentration of product: Tincture
• Therapeutic value of drug: Potent drug
• Cost of drug
• Solvent
The process of extraction can be divided into five
steps:
1. Size reduction of drug
2. Penetration of solvent into drug
3. Dissolution of constituents
4. Outward diffusion of solution from the drug
5. Separation of dissolved portion
Methods used for extraction:
1. Infusion
2. Decoction
3. Digestion
4. Percolation
5. Maceration
Infusion & Decoction:
Sr. No. Infusion Decoction

1. Cold or boiling water is used Drug is boiled in water.

as menstruum.
2. Drug having soft tissue is used. Drug having hard tissue is used.

3. Drug constituents may be Drug constituents should be non

volatile. volatile.

4. Final volume is adjusted. Final volume is not adjusted.

5. When boiling water is used as No such precaution is required.

menstruum, precaution are
taken to prevent the escape of
heat by covering the vessel
with a cloth .
 Infusion
This method is only applicable for soft drugs and drugs
containing water-soluble constituents
15-20 mins
Drug+ H2O filtrate

The filtrate is called infusion.

Heat is not applied.

Infusion should be used within 24 hours.

20-25% ethanol is used as a preservative.

 Decoction
This method is applicable for water soluble and
heat stable drugs obtained from hard and woody
sources.

15-20 mins
Drug +H2O filtrate
heat

The filtrate is called decoction. It should be used

within 24 hours.
 Maceration

In this method, the plant material is soaked in the

solvent.

The extraction time can vary from several minutes

up to weeks.

Gums, resins, oleo-gum resins etc., can be

extracted.
This method of tinctures production is officially

used in the case of resins, balsams, gums, soap,

etc., where the practical difficulties likely to be

encountered in percolation would offset any

advantages that the latter process might possess.

 Stages of the maceration:
1. Loading of crushed PRM with the prescribed volume of
extragent in the tank for maceration and allowed to stand
at room temperature 15 – 20 °C, with frequent agitation .
If there are not special instructions, the infusion continues
during 7 days.
2. The mixture then is strained, the marc (the damp solid
material) is pressed, washing raw by a small volume of
extragent, wring out again.
3. Flowing together all infusions and communicating by
solution for extraction to the desired volume.
4. The combined liquids are clarified by filtration or
decantation after standing.
 Maceration
The drug is placed with the whole of the menstruum
in a closed vessel for 2-7 days with occasional
shaking. After 2-7 days the liquid is removed &
marc is pressed.
Examples are: Tincture of orange, Tincture of squill.
Maceration process is divided into two types:
1. Modified maceration
2. Multiple maceration
Modified maceration:
• It is essentially used for extracting unorganized drugs.
Ex: gums, resins etc.
• This process is quick because the soluble constituents
are directly exposed to menstruum due to lack of
cellular structure.
• The final product is adjusted to definite volume.
• The filtrate should be collected in a dry receiver or in a
receiver rinsed with menstruum because the resinous
matter present in most of the unorganized drugs is
insoluble in water affecting the clarity of the final
product.
Ex: preparation of tincture of opium.
Multiple maceration:
• Multiple maceration is aimed at achieving maximum
extraction by using portions of total volume of menstruum
for successive maceration.
• The drug: menstruum ratio is low.
• The volume of menstruum for each maceration can be
calculated as follows,
For double maceration,
Volume of menstruum (total volume - vol.retained drug)/2 +
for 1st maceration = vol. retained by drug.
For triple maceration,
Volume of menstruum For 1st maceration = (total volume –
vol. retained by drug)/3 + vol. retained by drug
 Disadvantages of maceration:
this method is slow, raw material is not fully
exhausted.
Methods to intensify the maceration:
1. Repeated maceration (bismaceration)
2. Maceration with forced circulation of
extragent
3. Vortex extraction (turboextraction)
4. Ultrasound maceration
5. Maceration in the medium of milling (bolls
mill and rotating pulsation apparatus are used)
Maceration with circulation of the extragent.

It is performed in the tank 1 for maceration

with a perforated bottom 3, on which there
is the filter material 2.
4 – pump.
Solution for extraction (extragent) is smoothed
through PRM which is on perforated bottom
by the pump (4) for the several times to
achieve the equilibrium.
 Digestion

Modified form of maceration.

Solvent action is enhanced by heat

application

Suitable for heat stable drugs.

 Digestion

• is the form of maceration which consists in the

application of a gentle heat to the substance which is
being treated.
• It is used in those cases where a moderately elevated
temperature is unobjectionable; the heat increases the
solvent powers of the menstruum.
• If the solvent or menstruum is volatile it is necessary
to attach a reflux condenser to the vessel in which the
lotion is being conducted so that the solvent may be
recovered and returned.
Percolation:
The plant material is continuously flushed with
fresh solvent.
The extraction is continued until sufficient
compound is extracted.
 Percolation (from Lat. Rercolatio - filtering
through) is the method obtaining of extracts
while simultaneous loading of the extragent and
pouring out of the extract.
Stages of the Percolation:
1. Moistening of plant raw material (swelling materials), 4-
8 hours
2. Infusion, 24-48 hours
3. Obtaining the extract by simultaneous loading the
extragent and pouring out of the extract.
Percolator (a narrow, cone shaped vessel open at both ends)
is used.
Percolation:
Percolation process is divided into four types:
1. Continuous hot percolation
2. Simple percolation
3. Reserve percolation
4. Modified percolation
Continuous hot percolation: soxhlet
extraction
• Continuous hot percolation process or Soxhlet
extraction Apparatus.
• The apparatus consists of three parts-
A flask: For boiling of solvent.
A Soxhlet extractor: Having the drug in thimble, a
side tube & siphon tube
A reflux condenser: For condensation of vapors
In soxhlet extraction, similar
to percolation, the plant
material is continuously
flushed with fresh solvent.
But the fresh solvent
containing the extracted
analytes.

Thus, in contrast to
percolation, the total amount
of solvent is limited. Soxhlet
apparatus
Percolators
Simple percolation:
It involves 5 steps
1. Powdering of the drug
2. Imbibition of the drug with a little menstruum for 4 hours
3. Packing up to 2/3rd capacity of the percolator
4. Maceration: Sufficient menstrum is added allowed to saturate the
drug. When the drops start to come down through the nozzle, the
nozzle is closed and the moistened drug allowed to stand for 24
hours.
5. Percolation: The percolate is collected drop wise. The process is
continued till complete extraction has taken place.
Reserved percolation:
Here 3/4th of the percolate is collected and
reserved .
The final 1/4th of the percolate is then collected,
evaporated to syrupy
consistency and added to the reserved 3/4th
portion of the percolate.

Advantage:
Can be used to prepare concentrated liquid
extracts.
 Modified Percolation process:

Drug Imbibition Maceration Percolation & collect

1000 g for 4 hrs for 24 hrs 100 ml percolate

Maceration Percolation & collect

for 24 hrs 100 ml percolate
Maceration Percolation & collect
for 24 hrs 100 ml percolate
This process is continued in case drug is not completely exhausted.
The success of the process of percolation largely
depends on the regulation of the flow of the
percolate; if this is too rapid, incomplete exhaustion
will result, but if too slow, valuable time is wasted and
considerable loss of menstruum occurs from
evaporation.

For fluid extracts using 1000 Gm. of powder, and rate of

flow should not exceed 10 drops a minute; for official
quantities of tinctures and preparations of about the
same strength, 20 drops a minute
 Types of extraction
The extraction of the drug can be done by five methods:
1. Infusion
2. Decoction
3. Digestion
4. Maceration
5. Percolation
 TINCTURES.
Methods of preparation of
tinctures.
 Tinctures
are referred to galenicals obtained by extraction
of plant raw material (crude drugs) with an
appropriate solvent.
• The main object of manufacturing process is
separation of the soluble principles from drugs
by treating them with a liquid capable of
dissolving them, which is called the
menstruum or extragent.
 Tinctures
– is a liquid alcohol or water-alcohol extract are
obtained from dried or fresh plant or animal
raw materials, while production of which heat
and removal of the solution for extraction are
not carried out.
At the manufacture of tinctures from 1 mass part
of PRM (percolation resistance measurement
(PRM)) you can produce 5 volume parts of
finished product, from a potent drug – 10 parts.
 Advantages of tinctures

• Ethanol is able to dissolve substances which are

less soluble in water, while at the same time the
water content can dissolve the substances less
soluble in ethanol.
• It is possible to vary the proportion of ethanol
and water to produce tinctures with different
qualities because of different substances.
• The solvent also acts as a preservative.
 Tinctures

Simple Complex

mixture of extracts from

is derived from one
several plants, sometimes
type of HRM with the addition of drugs
 Methods obtaining of tinctures

1. Maceration and its improved types

2. Percolation
3. Dissolution of soft and dry extracts
(Direct method)
4. Other methods (Vortex extraction,
Ultrasonic, moistening, infusion)
Methods 1 and 2 have already
been discussed above.
 Vortex extraction
or turboextraction, is based on using of turbine
stirrer which is rotates with speed about 8000
– 13 000 times for 1 minute.
Turbine stirrer causes very intensive mixing of
raw material with the extragent and crushing
of raw material.
Extraction time is shortened to 10 min.
 Ultrasonic extraction.

The procedure involves the use of ultrasound

with frequencies ranging from 20 kHz to 2000
kHz; this increases the permeability of cell walls
and produces cavitation.

Source of ultrasound is attached to the body of

the tank and immersed in the medium of the
extraction.
Pressure with variable, cavitation and "wind
sound“ are created due ultrasound.
 Moistening
The solid ingredients are moistened with an
appropriate amount of the specified
menstruum and allowed to stand for
approximately 4 h in a well-closed container,
after which the mass is packed and the top of
the percolator is closed.
 Infusion
Additional menstruum is added to form a
shallow layer above the mass, and the mixture
is allowed to macerate in the closed percolator
for 24-48 h.
Raw material is poured over with the extragent
to create a "mirror” - thickness layer of
solution above the raw material which should
be 30 - 40 mm.
 Obtaining tinctures
The inlet and outlet of the percolator are opened
and the liquid contained therein is allowed to
drip slowly and additional menstruum is added
as required, until the percolate measures about
three-quarters of the required volume of the
finished product.

The mixed liquid is clarified by filtration or by

standing followed by decanting.
 Clarifing of extracts
Extracts are a muddy liquid, containing a
significant amount of suspended particles.
Extracts are clear by standing at above 10 °C to
obtain of a transparent liquid.
After standing more than 2 days they are filtered
by decantation (without shaking sediment).
Filterpress, Drook filters, Nootch filters,
centrifuges are used for filtration.
Dissolution of soft or dry extracts
1. Calculated amount of dry or soft extract is
dissolved in alcohol with required concentration
in a reactor with stirrer.
2. The obtained tinctures are filtered.

This method is characterized by a significant

reduction in the time of tinctures obtaining. It is
very simple, are used in a small number of
equipments.
• The tincture is prepared by dissolving or
diluting an extract, using alcohol of
appropriate concentration.
• The content of alcohol and constituents or,
where applicable, the content of alcohol and of
dry residue correspond to that of tinctures
obtained by maceration or percolation.
 Quality control
1. Appearance. Color, odor, opacity of the tincture are to be tested.
2. Relative density. Where applicable, the tincture complies with the
limits prescribed in the monograph.
3. Ethanol content. The ethanol content complies with that
prescribed. It's determined by distillation method.
4. Methanol and 2-propanol. Not more than 0.05 per cent.
5. Dry residue. Where applicable, the tincture complies with the
limits prescribed in the monograph.
6. Identity. This test is carried out by chemical reactions (assays) and
by chromatography
7. Quantitative determination of BAS.
8. Heavy metals. Not more than 0.001%.
9. Microbiological purity.