EXTRACTION PROCESSES

Prepared by: Dr .Rahila Bano

Assistant Professor
Pharmaceutics, DCOP, DUHS
CONTENTS

 Maceration
 Percolation
 Liquid-liquid extraction
 Large scale extraction
EXTRACTION

 It define as the treatments of plant and animal tissues with

solvents, where by the medicinally active constituents are
dissolved and most of the inert matter remains undissolved.

 Removal of soluble constituents from a solid or liquid or

semisolid with means of suitable solvents.

 Is the method of removal of a soluble fraction in the form of

a solution from an insoluble matrix with the help of a suitable
solvent.
GENERAL TERMS

 Menstrum:The solvents used for extraction

is menstrum

 Marc: Inert insoluble material that remains

after extraction

 Extractives:Concentrated preparations of
vegetable and animal drug obtained by
removal of the active constiteunts of the
respective drugs with suitable menstrum,
evaporation of all or nearly all solvent
NATURE OF MENSTRUM

 Polar: water, alcohol, acetone

 Non-polar: choloform, hexane, benzene, toluene,

diethyl-ether

 Non -polar solvents have dielectric constant is less

than 15
 CHOICE OF MENSTRUMS

The menstrum should have the following properties:

Highly selective and capacity of extractionfor the
compound to be extracted
Should not react with the extracted compound or any
other
Should have low price and easily available
Should be harmless to man and environment
Ease of evaporation at low heat
WATER(Menstrum)

 Is
a solvent for protein,coloring matter,
gums, glycosides, sugar, alkaloidal
salts,enzymes, many organic acids and
most of the organic salts.

Wax. fats, fixed oils and most alkaloids are

insoluble in water.
MERITS OF WATER

It is cheap

Non toxic

wild solvent action

Non-inflammable
DEMERITS OF WATER

Growing of mould and bacteria

Preservatives are required for extraction
Hydrolysis of many substances
Large amount of heat is required to
concentrate aqeous preparation than non-
aqeous preparation
ALCOHOL (Menstrum)

 Alcohol is a solvent for alkaloids, glycoside, volatile oil

and resins.

 Does not dissolve albuminous matter, gums, waxes, fats,

fixed oil and sugar
MERITS (ALCOHOL)

 The mould and bacteria can not grow in a solution in

which alcohol concentartion is 20% or more
 It is neutral and hence extraction products obtained
from its are compatible with other produts.
 A small amount of heat is required to concentrate the
alcoholic preparation.
 It is non-toxic in the concentration mostly present in
the preparations.
DEMERITS

 The preparation becomes costly when alcohol is used as

solvent for extraction of API.

 Flammable
ACETONE

Acetone dissolves many hydrophilic and lipophilic

components from the plants used, is miscible with
water
Volatile
Very useful solvent especially for antimicrobial
studies
where more phenolic compounds are required to
be extracted
MERITS and DEMERITS

 Prevent microbila contamination

 costly
 physiologically effected
 unsuitable for internal administration
OBJECTIVES OF EXTRACTION

 To obtain the therapeutic portion of dosage form from raw

materials and to eliminate the unwanted or inert material
by treatment with solvents
 They play a decisive role in the determination of
qualitative and quantitative composition of extracts.
 The extracts obtained are also utilized for the isolation
and charaterization of therapeutically active chemical
constiteunts
TYPES OF EXTRACTION

 Liquid-liquid extraction

 Solid- liquid extraction

LIQUID -LIQUID EXTRACTION

 Liquid-liquid extraction, also known as solvent extraction

and partitioning.
 It is a method to separate compounds based on their
relative solubilities in two different immiscible liquids,
ususally water and an organic solvent.
 It is an extraction of a substance from one liquid phase
into another liquid phase.
 is a basic technique-perfomed using a separtory funnel.
 In this technique, a solvent (known as
the extractive solvent) is brought in
contact with another solvents (termed
as the solute bearing solvent) in order
to bring the transfer of one or more
solute into the first solvent
 Separation of a substance from a
mixture by preferentially dissolving
that substance in a suitable solvent
 Solvent extraction is the most widely used method

 Th extraction of drug progresses through the following

stages:

Th solvent penetrates into the solid matrix

The solute dissolve in the solvents
The solute diffuse out the solid matrix
The extracted solute are collected
FACTORS AFFECTING EXTRACTION

Th properties of the extraction solvent

The physicochemical properties of drug

The particle size of raw materials

The solvent -to-solid ratio

The extraction temperature and duration

SOLID-LIQUID EXTRACTION

 Also called as leaching

 Th separation of soluble constituent from a solid by

extraction with a solvent

 It consist of two stages:

Contact of solute with the liquid phase
Separation of the liquid phase from solid phase
SELECTION OF EXTRACTION METHODS

Nature of the component

Nature of material to be used

Solvent system available

FACTOR AFFACTING CHOICE OF EXTRACTION PROCESS
 Character of drug

 Therapeutic value of drug

 Cost of drug

 Stability of drug

 Solvent (menstrum)

 Concentration of product
EXTRACTION PROCESSES LAY OUT
EXTRACTION METHODS

 Infusion

 Decoction

 Digestion

 Percolation

 Maceration
 INFUSION

It consist of pouring water over the drugs and

Then allowing to keep in contact with the water for the stated
period, usually 15 minutes, with occasional stirring and

Finally filtering off the liquid

INFUSION
TYPES OF INFUSION

 Fresh infusion

 Concentrated infusion
FRESH INFUSION

 Frsh infusion is an aqueous solution of active constituents

of a vegetable drug prepared by the process of infusion.

 Water is used as a menstrun because it has more

penetration powder and dissolves the API.

 According to pharmacopeia fresh infusion should be used

within 12hrs after it preparation because it get spoiled due
to microbial growth.
CONCENTRATED INFUSION

 Concentrated infusion are 8 time stronger than fresh

infusion
 Alcohol in the conc.of 20-25% is used as menstrum
 Hence these prepartion can be stored for longer period of
time (due to preservative action of alcohol)
 Eg. quassia (extraction of bark of tropical trees and used
as a insecticide)
DECOCTION
Drug is boiled with water for stated period usually 10 min

After boiling the liquids is strained and water is passed through the
content of the stainer to make the required volume

This process is mainly used for vegetable drugs of hard and woody
nature having thermostable water soluble constituents
DECOCTION
Digestion

The drug is extracting by heatig at particular pressure

This will increase the penetration power of the menstrum,

so that there is complete extraction of drug

Precaution should be taken so that increased temperature

may not harm the active constituents of the drug
 The apparatus known as ‘digestor’ is used for extraction
of drug by this method

 The whole of the drug along with the menstrum is placed

in the body of the digestor

 Place the cover over it and bolt it with the help of nuts

 The drug is treated with menstrum for a definite period

under specified condition of temperature and pressure
MACERATION (TYPE OF MACERATION)

Simple maceration (organised drug)

Maceration with adjustment (unorganised drug)

Multiple maceration (Double and triple

maceration)
SIMPLE MACERATION
 Drug is placed with the whole of the menstrum in a closed
vessel for seven days

 During this period shaking is done ocassionally

 After seven days, the liquid is strained and marc is pressed

 The expressed liquid is mixed with strained liquid

 It is then filtered to make a clear liquid

EXAMPLES

 Tincture of orange

 Tincture of lemon

 Tincture of squill
MACERATION WITH ADJUSTMENT

Unorganised drug is placed with 4/5th of the menstrum in a

closed vessel for period of 2-7 days

Shaking is done ocassionally

After stated period, liquid is filtered and final volume is

made up by passing remaining 1/5th menstrum. the marc is
not pressed
EXAMPLES

 Tincture of tolu

 compound tincture of benzoin

MACERATION PROCESSES FOR ORGANISED AND UNORGANISED DRUG

The process of maceration for organised and unorganised drug are

slightly differ as indicated below
Processes for organized drug Processes for unorganized drug
eg. (barks, root) eg.(gum,resin)
Drug + whole of menstrum Drug + 4/5th (in most cases) of
menstrum
Shake occasionally during 7 days Shake occasionally during 2-7 days as
specified

Strain of liquid, press the marc Decant the liquid, marc not pressed
Mix the liquid, clarify by subsedence Filter the liquid and pass more
for filteration menstrum through filter to volume
eg.tincture of squill eg. compound tincture of benzoin
MULTIPLE (DOUBLE AND TRIPLE MACERATION)

 Maceration process is carried out in the same way as

simple maceration process

 But the menstrum used is divided intotwo parts in double

maceration and into three parts in triple maceration
DOUBLE MACERATION PROCESS
 Drug is macerated twice by using the menstrum which is divided into parts in
such a manner that the same volume is used for each maceration
 The whole of the drug is macerated for 48hrs with quantity of menstrum
required for 1st maceration
 Strain the liquid and press the marc
 Macerated again for 24hrs with remaining menstrum required for second
maceration
 Strain the liquid and press the marc
 Mix the liquid obtained from two maceration and allow it to stand for 14 days
and then filter.
 Eg. Concentration infusion of orange, concentrated compound infusion of
gelatin
TRIPLE MACERATION PROCESS
 The whole of the drug is macerated for one hour with a part of
menstrum required for first, second and third maceration and
strained
 Press the marc lightly
 Then combine the liquid obtained from third, second and first
maceration
 Add alcohol 90% equal to 1/4th of the volume of the finished
product
 Allow it to stand for 14days and filter
 Eg. liquid extract of senna
PERCULATION

 Per means through

 Colare means to strian

 The process inwhich a communicated drug is extracted of

its soluble constituents by the slow passage of suitable
solvent through a column of drug
PERCOLATION

 Various percolation processes have been used for the

extraction of drugs:

Simple percolation
Percolation process for concentrated preparation
Reverse percolation process
Modified percolation process
Continuous hot paerculation or soxhelation
SIMPLE PERCULATION PROCESS

Three type of perculator are

used:

 Conical
 Cylinderical
 Steam jacketed
SIMPLE PERCULATION METHOD

 Simple perculation method are used for preparation of

tincture:

Comminution of drug
Imbibition of drug
Packing
Maceration
perculation
COMMINUTION

 It is the size reduction of drug usually from coarse powder

to fine powder so that:

To increase surface area

To insure completely removal of drug
To slow down the moment of menstrum
To uniform packing
IMBIBITION

 Swelling of drug by absorbing menstrum. It is

allow to stand for 4 hrs in a close container

 It is done to achieve following objectives:

To remove air

To avoid choking (difficulty in movement)
To avoid wasing out of fine particles
PACKING

 After imbibition drug is evenly packed into the

perculator
 Then a filter paper is placed on a bottom to support
the column of drugs
 The moistened drug is placed on the filter paper over
the moistened drug another filter paper is placed
having weight on it
 Then menstrum is added, close the lid if menstrum is
volatile.
MACERATION

 After packing sufficient menstrum is added and cover with

lid

 When liquid being to drop the lower orifice is closed

 Then perculator aside at 24hrs

PERCULATION

 After 24hrs orifice is open and mentrum is collected with a

controlled speed until 3/4th of menstrum is collected
 Then more menstrum is added and collected from the
lower orifice so that marc doesnot become dry
 The marc is pressed to get extract which is combine with
previous liquid
 Then it is allow to stand and then it is filtered
EXAMPLES OF SIMPLE PERCULATION

 Tincture of belladonna

 Compound tincture of cardamon

 Strong ticture of ginger

PERCULATION PROCESS FOR CONCENTRATED
PREPARATION
 Perculation processes for concentrated preparation are
used for liquid extract and solid extract

 Various method are used for preparaing concentartion

preparation:
Reserve perculation method
Modified perculation methd
RESERVE PERCULATION PROCESS

 In this method the first portion (3/4) portion of perculate

contains maximum amount of active constituent (70-80%) is
reserve as such
 The last portion of perculate (about 1/4th) is collected
separately and menstrum is evaporated to get syrup
consistency and mix with reserved perculate
 Final volume is adjusted by adding more menstrum, usually
alcohol is used as menstrum for reserve perculation
 Eg. liquorice liquid extract
MODIFIED PERCOLATION PROCESS

 In perculation process for preparation of tincture the

drug /perculate ratio is about 1:4
 The d/p ratio is reduce 1:3 by modifying perculation
process and hence there is lot of saving in heat, time and
menstrum
 Perculation is a displacement process
 The strong solution of active constituents of drug formed
during maceration is displace by fresh menstrum when
perculation started
 It is proved that stationary menstrum (menstrum remain in
contact with drug) dissolves more matter than flowing
menstrum
 Hnece more menstrum is required to exhaust the drug
when simple perculation process is used.
 But if continuous perculation stage has suitable breaks by
short maceration stages,the d/p ratio can be reduce to 1:3
CONTINUOUS HOT PERCULATION

 When active constituent of the drugs are not freely

soluble in the solvent or difficult to be displace from the
cell of the drug than it become necessary to extract the
crude by the action of hot menstrum for considerable
length of time.
 The fixed oil from seed and alkaloids from the drug are
extracted by continuous hot perculation process using
benzene, chloroform, petroleum, ether etc.
APPARATUS USED FOR HOT PERCULATION

 soxhlet apparatus used for

continuous hot
perculation . it divided into
three parts
Flask
soxhlet extractor
Condenser
METHOD

The drug to be extracted is packed in a paper cylinder made

from a filter paper and it is placed in the body of soxhlet
extractor
 The solvent is placed in the flask and apparatus is then fitted
 When solvent is boiled on heating the flask, it gets converted
in vapours
 These vapours enter into condenser through the side tube
and get condense into hot liquid which fall on the column of
the drug.
 When extractor get filled with the solvents, the level of
syphon tube also raises upto its top.
 The solvent containing API in the syphon tube syphon
over and run into the flask, thus emptying the body of
extractor
 This altering of filling and emptying the body of extractor
goes on continuously
 This process is repeated until about 15 times for complete
exhausted of the drug.
LIMITATION OF CONTINUOUS HOT PERCULATION

 Physical characteristics of drug: The physical

character of a drug is such that it would block the soxhlet
apparatus in case it is used for its extraction by this
method

 Eg. opium, resin gum, orange peel etc.

 Solvent: only pure solvent and constant boiling mixture
are can be used for this process

 Chemical constituent of the drug:The process is

unsuitable for drugs having thermolabile active
constituents such as enzymes, alkaloids, antraquinone
derivatives etc.
LARGE SCALE EXTRACTION

 Circulatory extraction
 Multiple stage extraction
 Extraction battery
REFERENCES

 Extraction methods in organic analysis by alan J.Handley

 Solvent Extraction: Classical and Novel Approaches by

Vladimir S Kislik