EXTRACT PREPARATION

Grinding/size reduction
• The first operation for manufacture of a simple preparation
that must be performed is grinding of the plant material to
a powder of suitable particle size.
• The particles have to be as uniform size as possible.
• Excessive dust can clog percolators and result in a turbid
extract which is hard to clarify.
• Large particles take a longer time for complete extraction
than small ones.
• Large differences in particle size thus slow down the
extraction process.
Grinding/size reduction
 Grinding of crude drugs
Types of machines used for grinding crude drugs:

Hammer mill
a common type for
grinding crude drugs
 Grinding of crude drugs
Types of machines used for grinding crude drugs:

Knife mill
is useful for production of
low-dust powder of leaves,
barks and roots for
subsequent percolation or
maceration.
 Grinding of crude drugs
Types of machines used for grinding crude drugs:

Tooth mill
is used for production of very
fine powders
 Grinding of crude drugs
Notes:
• Grinding produces a certain amount of heat which
must be observed when grinding crude drugs
containing heat-sensitive compounds.
• Mills cooled with liquid nitrogen are available for
such purposes.
• Cold grinding is also preferable for crude drugs
containing volatile oils.
• Following grinding, the material must be sifted to
ensure the proper particle size.
 Sifting of crude drugs
• Sieving
In sieving the material is passed through a sieve of
suitable mesh size giving two fractions.
The fraction passing the sieve consists of particles
with a size smaller than or corresponding to the
mesh size.
The remaining fraction consists of coarser
particles which are returned to the mill for
continued grinding.
 Sifting of crude drugs

• Blast sifting
In blast sifting the material to be classified is
blown with compressed air into an apparatus
which allows the particles to sediment according
to their weight.
Coarse, heavy particles settle fast whereas small,
light particles stay for a long time in the air stream
Sifting of crude drugs
 Extraction
as the term is used pharmaceutically,
involves separation of medicinally active portions
of plant or animal tissues from the inactive or inert
components by using selective solvents by
appropriate extraction technology.
The products so obtained are relatively impure
liquids, semisolids or powder intended only for
oral or external use.
 Extraction

MENSTRUM
Solvent used for extraction

MARC
The inert fibrous and other insoluble
materials remaining after extraction
 Extraction
GENERAL METHODS FOR EXTRACTION
1. Comminution (reducing particle size)
2. Penetration of the crude drug by menstrum
3. Dissolution of the chemical component by
menstrum
4. Diffusion of the dissolved chemical component
through the cell wall to the surrounding menstrum
5. Separation of the dissolved chemical component
from the marc by filtration or expression
 Extraction
Choice of solvent
As a general empirical rule:

 Non polar solvents (petroleum ether and hexane) will dissolve

non-polar compounds (fats and waxes).
While polar solvents (methanol, ethanol and water)
dissolve polar compound (alkaloid salts and sugars).
(that mean like dissolve like)
 The affinity of the solute for the organic phase may be
greatly increased by using mixture of solvents instead
of single ones
(sometimes used mixtures of solvent to increase the solubility).
 Extraction
Choice of solvent
Ideal solvent for certain pharmacologically active
constituent :
-Highly selective for that compound
-High capacity for the extraction
-Not react with all compound to be extracted
-Completely volatile
-Harmless
-Low price
 Extraction
Choice of solvent
Aliphatic alcohols with up to three carbon atoms, or
mixtures of the alcohols with water, are the solvents with
the greatest extractive power for almost all natural
substances of low molecular weight like alkaloids,
saponins and flavonoids.
According to the pharmacopoeias, ethyl alcohol is the
solvent of choice for obtaining classic extracts such as
tinctures and fluid, soft and dry extracts.
 Extraction
Choice of solvent
The ethanol is usually mixed with water to induce swelling of
the plant particles and to increase the porosity of the cell walls
which facilitates the diffusion of extracted substances from
inside the cells to the surrounding solvent.
For extraction of barks, roots, woody parts and seeds the ideal
alcohol/water ratio is about 7:3 or 8:2. For leaves or aerial
green parts the ratio 1:1 is usually preferred in order to avoid
extraction of chlorophyl
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COLD EXTRACTION
-Maceration
-Percolation
HOT EXTRACTION
-Decoction
-Infusion
-Sokhlet
-Distillation
ACCELERATED EXTRACTION
-Microwave assisted process
-Sonication
-Supercritical fluid
Extraction
 Extraction

MACERATION
a) Whole or coarsely powdered plant-drug is kept in
contact with the solvent in a stoppered container for a
defined period with/without frequent agitation until
soluble matter is dissolved
b) The mixture is strained, the marc pressed and the
liquid filtered.
 Extraction

PERCOLATION
a. The powdered drug is moistened with an
appropriate amount of the specified
menstruum
b. The moistened mass loosely packed in
percolator and covered
c. Additional menstruum added to give
shallow layer above the mass
d. Passing solvent through sample
e. Continuosly flow of solvent
f. Large volume of solvent used
 Extraction

INFUSION
Infusion is dilute solution of
the readily soluble
constituents of the crude drug
• Fresh infusion is prepared by
macerating the drug for a
short period of time with hot
(boiling) water
 Extraction

DIGESTION

It is like maceration but gentle heat is

used during the process of extraction
• It is employed when moderately elevated
temperature is not objectionable as the
solvent efficiency is increased
 Extraction

DECOCTION
Powdered drug is boiled in specified
volume of water for defined time,
cooled and strained or filtered
• Suitable for extracting water-
soluble, heat stable constituents
• Ratio of drug to water 1:4 or 1:16
which is brought down to ¼ of its
original volume by boiling
 Extraction
HOT CONTINUOUS EXTRACTION
(SOXHLET)
Large amount of drug can be extracted with
much smaller quantity of solvent procedure
on large scale.
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.
 Extraction
COUNTER CURRENT EXTRACTION (CCE)
• Raw material is moved in one direction
within a cylindrical extractor where it comes
in contact with the extracting solvent falling
against it.
• The further the starting material moves,
more concentrated becomes the extract
• Complete extraction possible with
optimization of quantities of solvent and the
material and their flow rates
• Process is efficient requiring least time
with no risk of high temperature
 Extraction
ULTRASOUND EXTRACTION (SONICATION)

frequencies ranging from 20 KHz to 2000

KHz increases permeability of cell wall to
produce cavitation
•Deleterious effect of ultrasound energy on
the active constituents of the medicinal plant
through formation of free radicals and
consequently in the drug molecules.
 Extraction
MICROWAVE ASSISTED PROCESS

H2O vibration
 Extraction
SUPERCRITICAL FLUID EXTRACTION

•The critical point of a pure

substance is defined as the highest
pressure and temperature at which
it exists in vapour-liquid
equilibrium
• At pressure and temperature
above this point, single
homogenous fluid which forms is
said to be supercritical
•A substance in supercritical phase is neither a true liquid
nor a true gas and has some properties of each
 Extraction
SUPERCRITICAL FLUID EXTRACTION
• Supercritical fluids can dissolve wide variety of organic
compounds and their solvent power can be raised near their
critical points by small pressure and temperature changes
• At high temperature and low pressure, the density is low
and the supercritical fluid behaves more like a gas. But at
low temperature and high pressure, the density is increase
and it assumes the properties of a liquid
• Supercritical carbondioxide (sCo) is considered to exist at
pressure above 73.8 bar (or atm.) and temp. above 31.20C
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Factors Affecting Choice of Extraction Process
The final choice of the process to be used for the extraction of a
drug will depend on a number of factors, including:

Character of Drug
If hard and tough (such as nux vomica) use percolation.
If ‘unpowderable’ (such as squill) use maceration.
If an ‘unorganized drug (such as benzoin) use maceration.
If preferable to avoid powdering (such as senna fruits) use
maceration.
Thus, knowledge of the pharmacognosy of the drug is
essential to selection of the extraction process that will give
the best result.s
 Extraction

Therapeutic value of the drug

When the drug has considerable therapeutic value, the

maximum extraction is required, so that percolation is used, as
in belladonna. If the drug has little therapeutic value, however,
the efficiency of extraction is unimportant and maceration is
adequate; for example, “flavours” (lemon), or “bitters”,
(gentian).

Stability of drug
Continuous extraction should be avoided when the constituents
of the drug are thermo-labile.
 Extraction
Cost of drug
From the economic point of view, it is desirable to obtain
complete extraction of an expensive drug, so that percolation
should be used; Ginger is an example of this type.
For cheap drugs, the reduced efficiency of maceration is
acceptable in view of the lower cost of the process. In
particular, the cost of size reduction to a powdered state is
avoided, whereas this is a significant part of the percolation
process.

Solvent
If the desired constituents demand a solvent other than a pure
boiling solvent or an azeotrope, continuous extraction should
be used.
 Extraction
Concentration of product
Dilute products such as tincture can be made by maceration or
percolation, depending on the previous factors.
For semi-concentrated preparations (concentrated infusions,
for e.g.) the more efficient percolation process is used) unless
the drug cannot be powdered or is not worth powdering, when
double or triple maceration is chosen.
Concentrated preparations, of which liquid extracts or dry
extracts are example, are made exclusively by percolation,
with the exception that continuous extraction can be used if
the solvent is suitable and the constituents are thermo-stable.
 Extraction

Recovery of solvent from the marc

The residue of the drug after extraction (often known as the
marc) is saturated with solvent and if economic the latter is
recovered
 Evaporation of extract

FREE EVAPORATION
: WATER BATH, HOT PLATE,
OVEN
 Evaporation of extract
UNDER REDUCED PRESSURE
: ROTARY EVAPORATOR
 Evaporation of extract
FREEZING
Lyophilization / freezed dryer
 Evaporation of extract

•Freeze drying is the process of removing water or other

solvent from a frozen product by sublimation.

• Conventional drying cause the material to shrink,

damaging the cells while in freeze drying process,
the solid components are held in place by rigid ice.
 Evaporation of extract

SPRAY DRYING
 Evaporation of extract
•SPRAY DRYING is the most widely used industrial
process involving particle formation and drying.

• Highly suited for the continuous production of dry

solids in either powder, granulate or agglomerate form
liquid feed stocks as solutions, emulsions and pump able
suspensions.

• Spray dryer involves the atomization of a liquid

feedstock into a spray of droplets and contacting the
droplets with hot air in a drying chamber.
 Evaporation of extract

N2 blow down
 Evaporation of extract

Fluid bed drying

 Evaporation of extract

Fluid bed drying