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Miss Harshada R. Bafna.
EXTRACTION PROCESSES
INTRODUCTION & DEFINITIONS
2
 It may be defined as the treatment of the plant or animal
tissues with appropriate solvent, which would dissolve the
medicinally active constituents.
 Menstrum: Solvent used for extraction (ex. water,
alcohol, ether, acetone, ethyl acetate)
 Marc: The inert fibrous and other insoluble materials
remaining after extraction
 Tinctures: are alcoholic or hydroalcoholic solutions
prepared from vegetable material or from chemical
substances. E.g. belladona tincture
8/5/2022
Extraction process (HRB)
 Solvents used for extraction process
The solvents used in extraction are capable of penetrating the
tissues of the drug and dissolve the active principles contained in its
cell.The various solvents used are water, propene, butane,
ethylacetate, ethanol, methanol, CO 2 , N 2 O, acetone etc.
Water
It is the cheap, non toxic, non inflammable and has wide solvent
action. Eg; proteins, glycosides, enzymes, sugar etc.
Disadvantages
• Water may promote growth of mould and bacteria, hence requires a
preservative.
• It may leads to hydrolysis.
• Large amount of heat is required to concentrate the aqueous
preparations.
• It promote fermentation or decomposition of the preparation
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Extraction process (HRB)
3
Alcohol
It is the important solvent for dissolves alkaloids, alkaloidal
salts, glycosides etc. it also dissolves many colouring matter,
tannins, etc. it doesn’t dissolve gums waxes, fats etc.
Merits
 It doesn’t allow the growth of mould and bacteria in above
20% of alcohol
 It is nontoxic in the concentration mostly present in the
preparations.
 Small amount of heat is requiered for concentration
Demerits
 Cost
 Inflammable, volatile etc
 Solvents such as ether, chloroform, light petroleum are rarely
used.
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Extraction process (HRB)
4
PROCESSES USED FOR EXTRACTION
5
SIMPLE
PERCOLATION
MACERATION
WITH
ADJUSTMENT
SIMPLE
MACERATION
MULTIPLE
MACERATION
PERCOLATION
PROCESS FOR
CONCENTRATED
PREPARATIONS
CONTINIOUS
PERCOLATION
PROCESS
RESERVE
PERCOLATION
PROCESS
MODIFIED
PERCOLATION
PROCESS
EXTRACTION PROCESS
INFUSION DECOCTION MACERATION PERCOLATION DIGESTION
CONCENTRATED
INFUSION
FRESH
INFUSION
8/5/2022
Extraction process (HRB)
INFUSION
6
 It involves pouring water over drugs and allowing it to keep in
contact with water for the stated period, usually 15 minutes, with
occasional stirring and finally filtering off the liquid.
 Marc is not pressed
 Boiling water commonly used as solvent
 After the specified time the liquid is filtered and dispense as
drug.
Short time is sufficient for extraction due to readily soluble
constituent of crude drug and its dilute property
e.g. Coffee pot or a teapot.
1. Fresh infusions –
In this aqueous solution of a active constituents of a vegetable
drug by the process of infusion.
e.g. fresh infusion of quassia.
Fresh infusions are liable to fungus and bacterial growth, and it is
necessary to dispense them within twelve hours of their
preparation. 8/5/2022
Extraction process (HRB)
7
2.Concentrated infusions are prepared by modified
percolation or maceration process.
8/5/2022
Extraction process (HRB)
DECOCTION
8
 In this process, the crude drug is boiled in a specified volume
of water for a defined time; it is then cooled and strained or
filtered. This procedure is suitable for extracting water-
soluble, heatstable constituents. The starting ratio of crude
drug to water is fixed, e.g. 1:4 or 1:16; the volume is then
brought down to one-fourth its original volume by boiling
during the extraction procedure. Then, the concentrated
extract is filtered and used as such or processed further.
• Example: Cinchona barkor wood
8/5/2022
Extraction process (HRB)
Comparison between infusion and decoction
Item Infusion Decoction
1- Plant Soft structure (ex. Senna
leaves)
Hard woody structure (ex.
Cinchona bark)
2- Menstrum Boiling or cold water Boiling water
3- Procedure Infusing the drug with cold or
hot water
Boiling the drug with
water
4- Time Calculated as soon as water is
added to drug
Calculated as soon as the
water begins to boil
5- Adjustment
of final volume
No adjustment Adjustment is necessary
6- Apparatus Infusion earthenware pot Any covered apparatus
7- Storage Used fresh within 12 hours Used fresh and when
stored in refrigerator used
within few days
9
8/5/2022
Extraction process (HRB)
DIGESTION
10
 Digestion is the process in which heat as well as pressure
is used for extraction.
 The equipment is like a pressure cooker or autoclave and
is called digester.
 Extraction of non-thermolabile materials is more efficient
in it because of high penetration power of solvent and
solubilisation rate of soluble matters of the crude drug
due to high pressure and temperature respectively
8/5/2022
Extraction process (HRB)
MACERATION
11
Various types of maceration process are
 Simple Maceration: A process for tinctures made from
organized drug e.g. roots, stems, leaves etc.
 Maceration with Adjustment: A process for tinctures made
from unorganized drugs such as oleo resins and gum resins.
 Double Maceration and Triple Maceration Process: for
concentrated preparations.
8/5/2022
Extraction process (HRB)
Maceration
12
Plant material (crushed or cut
small or moderately coarse
powder)
Placed in a closed vessels
Menstruum added (whole)
Allowed to stand for 7 days
shaking occasionally
Liquid strained off
Solid residue (marc)pressed
(recover as much as occluded)
(Strained and expressed liquids
mixed)
Clarified by subsidence and
filtration
Evaporation and concentration
8/5/2022
Extraction process (HRB)
SIMPLE MACERATION
13
• Drug is placed in wide mouthed container which can be well
stoppered to prevent the evaporation of menstruum which is
mostly concentrated alcohol.
• The drug is placed with the whole of the menstruum in a closed
vessel for 7 days
• During this period shaking is done occasionally
• After 7 days liquid is strained and marc is pressed – in filter
press, hydraulic press or hand press, squeezed in muslin piece
etc.
• Then filtered to make a clear liquid.
• The final volume is not adjusted.
• E.g. tincture of orange, tincture of lemon
8/5/2022
Extraction process (HRB)
MACERATION WITH ADJUSTMENT
14
 The unorganized drug is placed with 4/5th of menstruum in a
closed vessel in a closed vessel for a period of 2-7 days
 Shaking done occasionally
 After the stated period, the liquid is filtered and the final
volume is made up by passing the remaining 1/5th of the
menstruum through the filter
 The marc is not pressed
 E.g. tincture of tolu, compound tincture of benzoin
8/5/2022
Extraction process (HRB)
DOUBLE MACERATION
15
 The drug is macerated twice with the menstruum which is
divided into two equal volume.
Where
 V1 is volume of menstruum required for first maceration
Vt is total volume of menstruum
Vr is volume of menstruum to be retained by drug or marc
 Volume required for 2nd maceration is the difference between
Vt and V1
 Vr is determined by performing trial to get volume retained by
known weight of drug
MULTIPLE MACERATION
8/5/2022
Extraction process (HRB)
16
 The whole of the drug is macerated for 48 hours with the quantity
of menstruum required for first maceration.
 Strain the liquid and press the marc.
 Macerate again for 24 hours with the remaining menstruum
required for second maceration
 Strain the liquid and press the marc.
 Mix the liquids obtained from two macerations and allow it to
stand for 14 days and filter.
 E.g. concentrated compound infusion of Chirata, concentrated
compound infusion of Gentian
8/5/2022
Extraction process (HRB)
TRIPLE MACERATION
17
 In this process, the drug is macerated thrice by using menstruum
which is divided into 3 parts in such a manner that same volume is
used for each maceration.
 Volume of menstruum required by the first maceration=
Total vol. of menstruum – vol. to be retained by the drug + Vol. to be retained by
drug
3
 Volume of menstruum required by the second maceration=
Total volume of menstruum - vol. of menstruum used in first maceration
2
8/5/2022
Extraction process (HRB)
18
 The whole of the drug is macerated for 1 hr with a part of
menstruum required for first maceration and strained.
 Macerate again for 1 hr with a part of menstruum required for
2nd maceration and strained.
 Macerate again for 1 hr with a part of menstruum required for
3rd maceration and strained.
 Press marc lightly then combine the liquid obtained from 2nd
and 3rd maceration and evaporate it to a specific extent
8/5/2022
Extraction process (HRB)
19
 Mix it with the liquid obtained from 1st maceration
 Add alcohol 90% equal to 1/4th of the volume of the finished
product
 Adjust volume with water.
 Allow to stand for 14 days and filter
 E.g. concentrated infusion of Quassia, liquid
 extract of Senna
8/5/2022
Extraction process (HRB)
PERCOLATION
20
1. Simple percolation or percolation process for
tinctures.
2. Percolation processes for concentrated preparations
such as:
i. Reserve percolation process
ii. Modified percolation process
3. Continuous hot percolation or Soxhelation
PERCOLATION – APPARATUS
• Conical percolator
• Cylindrical percolator
• Steam jacketed percolator
8/5/2022
Extraction process (HRB)
21
Fig: Simple percolator
8/5/2022
Extraction process (HRB)
SIMPLE PERCOLATION
22
 There are three stages in the official method for preparation of
tinctures by percolation process
1. Imbibition:
 powdered drug is moistened with a sufficient quantity of
menstruum and allowed to stand for 4 hours in a closed vessel.
 It is done inorder to allow swelling of the tissues before
packing into the percolator.
 Dry powder if packed into percolator may cause blockage of
the percolator.
 It allows entrapped air to escape, dry powder drug would
have air entrapped within them, this may resist the flow of
Menstrum and will disturb the packing of the powdered drug.
8/5/2022
Extraction process (HRB)
23
 Prior to packing of the imbibed drug into percolator uniformity of
particle size is ensured by passing the moistened mass through a sieve
of coarse aperture.
 Glass wool moistened with solvent is kept at the bottom to avoid
blockage of outlet or tap. Cotton wool may not be used as after getting
soaked it would also create a impermeable mass.
 The imbibed drug is packed in the percolator upto 2/3rd or 3/4th of the
volume of percolator.
 Filter paper is placed above this layer and above this a layer of sand is
placed inorder to prevent disturbance of top layer when the Menstrum
is added into the percolator.
 Sufficient quantity of menstruum needs to be added to saturate the
material.
 When the liquid starts coming out of the percolator outlet is closed and
add Menstrum forming a layer of solvent above the imbibed mass.
8/5/2022
Extraction process (HRB)
24
2.Maceration:
 The moistened drug is left in contact with menstruum for 24
hrs.
 During this period, menstruum dissolves the active
constituent of the drug and becomes almost saturated with
it.
3. Percolation
 It consists of the downward displacement of the saturated
solution formed in maceration and extraction of the
remaining active constituents present in the drug by the
slow passage of the menstruum through the column of the
drug.
8/5/2022
Extraction process (HRB)
25
 After collecting 3/4th of the required volume of the finished
product or when the drug is completely exhausted, the marc
is pressed.
 Mix the expressed liquid with percolate.
 Add sufficient quantity of menstruum to produce the
required volume and then filter.
E.g. tincture of belladona, compound tincture of cardamom,
strong tincture of ginger.
8/5/2022
Extraction process (HRB)
PERCOLATION PROCESS FOR CONCENTRATED
PREPARATIONS
26
 Used to prepare liquid extracts and solid extracts.
 Types of processes are:
 Reserve percolation process
 Modified percolation process
8/5/2022
Extraction process (HRB)
1. Reserved Percolation Process
27
• In this process, a part of percolate, usually 3/4th of the volume of
the finished preparation, is reserved (first percolate) containing
high solute concentration.
• Percolation process is continued till the drug is completely
exhausted.
• The percolate thus receives contains traces of active constituents
of the drug.
• Evaporation or distillation is done to recover the costly
menstruum.
• Hence, the major portion of the active constituents of the drug are
saved from detorioration.
• The remaining soft extract is then added to reserve percolate.
• Volume make up is done using menstruum.
8/5/2022
Extraction process (HRB)
2. MODIFIED PERCOLATION PROCESS
28
• In percolation process, the drug/percolate (d/p) ratio is about 1:4,
the d/p ratio is reduced to 1:3 by modifying the percolation
process and hence there is a lot of saving in heat, time and
menstruum.
• Percolation is the displacement process.
• The strong solution of active constituents of drug formed during
maceration is displaced by the fresh menstruum when percolation
process is started.
• Menstruum remaining in contact with the drug dissolves more
matter than the flowing menstruum.
8/5/2022
Extraction process (HRB)
29
• Hence, more menstruum is required to exhaust the
drug when simple percolation process is used.
• In simple percolation process:
Drug Imbitition Maceration percolation and
collect the percolate, i.e. ¾ of the volume of the
finished product.
In modified percolation process:
Drug-imbibition-maceration-percolation and collect 1000ml of percolate
(24hr)
-maceration-percolation and collect 1000ml of percolate
(12hr)
-maceration –percolation and collect 1000ml of percolate
(12hr)
Drug:percolate
1000gm:3000ml
d/p=1:3
8/5/2022
Extraction process (HRB)
30
 After exhaustion of the drug, the percolate is evaporated
and then mixed with the main percolate.
 The final volume is made by adding more of menstruum.
8/5/2022
Extraction process (HRB)
Continuous hot percolation process or soxhlet extraction or
soxhleation
31
 When active constituents of the drug are not freely soluble in the
solvent or difficult to be displaced from the cells of the drug, then it
becomes necessary to extract the crude drug by action of hot
menstruum for a considerable length of time.
 The fixed oils from seeds and alkaloids from the drug are extracted
by continuous hot percolation process using benzene, chloroform,
petroleum, ether etc.
Soxhlet apparatus
1. Flask containing the boiling water
2. Soxhlet Extractor: in which the drug to be extracted is packed.
 It has a side tube which carries the vapors of the solvent from
the flask to the condenser and a siphon tube which siphons
over the extract from soxhlet extractor to the flask.
 A condenser in which the vapors of the solvent are condensed
again into solvent.
8/5/2022
Extraction process (HRB)
Soxhlet apparatus
32 8/5/2022
Extraction process (HRB)
33
PROCEDURE
 The drug 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
 The apparatus is then fitted as shown is figure.
 When solvent is boiled on heating flask, it gets converted into
vapors.
 These vapors enter into the condenser through the side tube and
get condensed into hot liquid which falls on column of the drug.
 When the extractor gets filled with the solvent, the level of
siphon tube also raises up to its top.
8/5/2022
Extraction process (HRB)
34
 The solvent containing active constituents in the siphon tube
siphon over and run into the flask, thus emptying the body of
extractor.
 This alteration of filling and emptying the body of extractor goes
on continuously until the drug is exhausted (normally 15 times).
 The soluble active constituent of the drug remain in the flask
where solvent is repeatedly volatilized.
8/5/2022
Extraction process (HRB)
Factors affecting the choice of extraction process
35
1. Character of drug
Knowledge of pharmacognosy – maceration process if drug is
soft, percolation process used when drug is hard and tough
2. Therapeutic value of the drug:
when the drug has high therapeutic value, maximum extraction is
required, so percolation process is used e.g. Belladona.
3. Cost of drug
costly drugs are extracted by percolation process, whereas cheap
drugs are extracted by maceration process.
4. Stability of drug:
-Thermolabile drugs-maceration or percolation should be done.
- No hot extraction process should be carried out.
8/5/2022
Extraction process (HRB)
36
5. solvent:
 Maceration process recommended-if water is used as solvent.
 Percolation process-nonaqueous solvents.
6. Concentration of product –
• The dilute products such as tinctures can be made by using
maceration or percolation process, depending on other factors.
• For semi-concentrated preparations, such as concentrated
infusions, double or triple maceration process can be used.
The liquid extracts or dry extracts or dry extracts which are
concentrated preparations are prepared by using percolation
process.
8/5/2022
Extraction process (HRB)
8/5/2022
Extraction process (HRB)
37

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extraction processes.pptx

  • 1. Miss Harshada R. Bafna. EXTRACTION PROCESSES
  • 2. INTRODUCTION & DEFINITIONS 2  It may be defined as the treatment of the plant or animal tissues with appropriate solvent, which would dissolve the medicinally active constituents.  Menstrum: Solvent used for extraction (ex. water, alcohol, ether, acetone, ethyl acetate)  Marc: The inert fibrous and other insoluble materials remaining after extraction  Tinctures: are alcoholic or hydroalcoholic solutions prepared from vegetable material or from chemical substances. E.g. belladona tincture 8/5/2022 Extraction process (HRB)
  • 3.  Solvents used for extraction process The solvents used in extraction are capable of penetrating the tissues of the drug and dissolve the active principles contained in its cell.The various solvents used are water, propene, butane, ethylacetate, ethanol, methanol, CO 2 , N 2 O, acetone etc. Water It is the cheap, non toxic, non inflammable and has wide solvent action. Eg; proteins, glycosides, enzymes, sugar etc. Disadvantages • Water may promote growth of mould and bacteria, hence requires a preservative. • It may leads to hydrolysis. • Large amount of heat is required to concentrate the aqueous preparations. • It promote fermentation or decomposition of the preparation 8/5/2022 Extraction process (HRB) 3
  • 4. Alcohol It is the important solvent for dissolves alkaloids, alkaloidal salts, glycosides etc. it also dissolves many colouring matter, tannins, etc. it doesn’t dissolve gums waxes, fats etc. Merits  It doesn’t allow the growth of mould and bacteria in above 20% of alcohol  It is nontoxic in the concentration mostly present in the preparations.  Small amount of heat is requiered for concentration Demerits  Cost  Inflammable, volatile etc  Solvents such as ether, chloroform, light petroleum are rarely used. 8/5/2022 Extraction process (HRB) 4
  • 5. PROCESSES USED FOR EXTRACTION 5 SIMPLE PERCOLATION MACERATION WITH ADJUSTMENT SIMPLE MACERATION MULTIPLE MACERATION PERCOLATION PROCESS FOR CONCENTRATED PREPARATIONS CONTINIOUS PERCOLATION PROCESS RESERVE PERCOLATION PROCESS MODIFIED PERCOLATION PROCESS EXTRACTION PROCESS INFUSION DECOCTION MACERATION PERCOLATION DIGESTION CONCENTRATED INFUSION FRESH INFUSION 8/5/2022 Extraction process (HRB)
  • 6. INFUSION 6  It involves pouring water over drugs and allowing it to keep in contact with water for the stated period, usually 15 minutes, with occasional stirring and finally filtering off the liquid.  Marc is not pressed  Boiling water commonly used as solvent  After the specified time the liquid is filtered and dispense as drug. Short time is sufficient for extraction due to readily soluble constituent of crude drug and its dilute property e.g. Coffee pot or a teapot. 1. Fresh infusions – In this aqueous solution of a active constituents of a vegetable drug by the process of infusion. e.g. fresh infusion of quassia. Fresh infusions are liable to fungus and bacterial growth, and it is necessary to dispense them within twelve hours of their preparation. 8/5/2022 Extraction process (HRB)
  • 7. 7 2.Concentrated infusions are prepared by modified percolation or maceration process. 8/5/2022 Extraction process (HRB)
  • 8. DECOCTION 8  In this process, the crude drug is boiled in a specified volume of water for a defined time; it is then cooled and strained or filtered. This procedure is suitable for extracting water- soluble, heatstable constituents. The starting ratio of crude drug to water is fixed, e.g. 1:4 or 1:16; the volume is then brought down to one-fourth its original volume by boiling during the extraction procedure. Then, the concentrated extract is filtered and used as such or processed further. • Example: Cinchona barkor wood 8/5/2022 Extraction process (HRB)
  • 9. Comparison between infusion and decoction Item Infusion Decoction 1- Plant Soft structure (ex. Senna leaves) Hard woody structure (ex. Cinchona bark) 2- Menstrum Boiling or cold water Boiling water 3- Procedure Infusing the drug with cold or hot water Boiling the drug with water 4- Time Calculated as soon as water is added to drug Calculated as soon as the water begins to boil 5- Adjustment of final volume No adjustment Adjustment is necessary 6- Apparatus Infusion earthenware pot Any covered apparatus 7- Storage Used fresh within 12 hours Used fresh and when stored in refrigerator used within few days 9 8/5/2022 Extraction process (HRB)
  • 10. DIGESTION 10  Digestion is the process in which heat as well as pressure is used for extraction.  The equipment is like a pressure cooker or autoclave and is called digester.  Extraction of non-thermolabile materials is more efficient in it because of high penetration power of solvent and solubilisation rate of soluble matters of the crude drug due to high pressure and temperature respectively 8/5/2022 Extraction process (HRB)
  • 11. MACERATION 11 Various types of maceration process are  Simple Maceration: A process for tinctures made from organized drug e.g. roots, stems, leaves etc.  Maceration with Adjustment: A process for tinctures made from unorganized drugs such as oleo resins and gum resins.  Double Maceration and Triple Maceration Process: for concentrated preparations. 8/5/2022 Extraction process (HRB)
  • 12. Maceration 12 Plant material (crushed or cut small or moderately coarse powder) Placed in a closed vessels Menstruum added (whole) Allowed to stand for 7 days shaking occasionally Liquid strained off Solid residue (marc)pressed (recover as much as occluded) (Strained and expressed liquids mixed) Clarified by subsidence and filtration Evaporation and concentration 8/5/2022 Extraction process (HRB)
  • 13. SIMPLE MACERATION 13 • Drug is placed in wide mouthed container which can be well stoppered to prevent the evaporation of menstruum which is mostly concentrated alcohol. • The drug is placed with the whole of the menstruum in a closed vessel for 7 days • During this period shaking is done occasionally • After 7 days liquid is strained and marc is pressed – in filter press, hydraulic press or hand press, squeezed in muslin piece etc. • Then filtered to make a clear liquid. • The final volume is not adjusted. • E.g. tincture of orange, tincture of lemon 8/5/2022 Extraction process (HRB)
  • 14. MACERATION WITH ADJUSTMENT 14  The unorganized drug is placed with 4/5th of menstruum in a closed vessel in a closed vessel for a period of 2-7 days  Shaking done occasionally  After the stated period, the liquid is filtered and the final volume is made up by passing the remaining 1/5th of the menstruum through the filter  The marc is not pressed  E.g. tincture of tolu, compound tincture of benzoin 8/5/2022 Extraction process (HRB)
  • 15. DOUBLE MACERATION 15  The drug is macerated twice with the menstruum which is divided into two equal volume. Where  V1 is volume of menstruum required for first maceration Vt is total volume of menstruum Vr is volume of menstruum to be retained by drug or marc  Volume required for 2nd maceration is the difference between Vt and V1  Vr is determined by performing trial to get volume retained by known weight of drug MULTIPLE MACERATION 8/5/2022 Extraction process (HRB)
  • 16. 16  The whole of the drug is macerated for 48 hours with the quantity of menstruum required for first maceration.  Strain the liquid and press the marc.  Macerate again for 24 hours with the remaining menstruum required for second maceration  Strain the liquid and press the marc.  Mix the liquids obtained from two macerations and allow it to stand for 14 days and filter.  E.g. concentrated compound infusion of Chirata, concentrated compound infusion of Gentian 8/5/2022 Extraction process (HRB)
  • 17. TRIPLE MACERATION 17  In this process, the drug is macerated thrice by using menstruum which is divided into 3 parts in such a manner that same volume is used for each maceration.  Volume of menstruum required by the first maceration= Total vol. of menstruum – vol. to be retained by the drug + Vol. to be retained by drug 3  Volume of menstruum required by the second maceration= Total volume of menstruum - vol. of menstruum used in first maceration 2 8/5/2022 Extraction process (HRB)
  • 18. 18  The whole of the drug is macerated for 1 hr with a part of menstruum required for first maceration and strained.  Macerate again for 1 hr with a part of menstruum required for 2nd maceration and strained.  Macerate again for 1 hr with a part of menstruum required for 3rd maceration and strained.  Press marc lightly then combine the liquid obtained from 2nd and 3rd maceration and evaporate it to a specific extent 8/5/2022 Extraction process (HRB)
  • 19. 19  Mix it with the liquid obtained from 1st maceration  Add alcohol 90% equal to 1/4th of the volume of the finished product  Adjust volume with water.  Allow to stand for 14 days and filter  E.g. concentrated infusion of Quassia, liquid  extract of Senna 8/5/2022 Extraction process (HRB)
  • 20. PERCOLATION 20 1. Simple percolation or percolation process for tinctures. 2. Percolation processes for concentrated preparations such as: i. Reserve percolation process ii. Modified percolation process 3. Continuous hot percolation or Soxhelation PERCOLATION – APPARATUS • Conical percolator • Cylindrical percolator • Steam jacketed percolator 8/5/2022 Extraction process (HRB)
  • 22. SIMPLE PERCOLATION 22  There are three stages in the official method for preparation of tinctures by percolation process 1. Imbibition:  powdered drug is moistened with a sufficient quantity of menstruum and allowed to stand for 4 hours in a closed vessel.  It is done inorder to allow swelling of the tissues before packing into the percolator.  Dry powder if packed into percolator may cause blockage of the percolator.  It allows entrapped air to escape, dry powder drug would have air entrapped within them, this may resist the flow of Menstrum and will disturb the packing of the powdered drug. 8/5/2022 Extraction process (HRB)
  • 23. 23  Prior to packing of the imbibed drug into percolator uniformity of particle size is ensured by passing the moistened mass through a sieve of coarse aperture.  Glass wool moistened with solvent is kept at the bottom to avoid blockage of outlet or tap. Cotton wool may not be used as after getting soaked it would also create a impermeable mass.  The imbibed drug is packed in the percolator upto 2/3rd or 3/4th of the volume of percolator.  Filter paper is placed above this layer and above this a layer of sand is placed inorder to prevent disturbance of top layer when the Menstrum is added into the percolator.  Sufficient quantity of menstruum needs to be added to saturate the material.  When the liquid starts coming out of the percolator outlet is closed and add Menstrum forming a layer of solvent above the imbibed mass. 8/5/2022 Extraction process (HRB)
  • 24. 24 2.Maceration:  The moistened drug is left in contact with menstruum for 24 hrs.  During this period, menstruum dissolves the active constituent of the drug and becomes almost saturated with it. 3. Percolation  It consists of the downward displacement of the saturated solution formed in maceration and extraction of the remaining active constituents present in the drug by the slow passage of the menstruum through the column of the drug. 8/5/2022 Extraction process (HRB)
  • 25. 25  After collecting 3/4th of the required volume of the finished product or when the drug is completely exhausted, the marc is pressed.  Mix the expressed liquid with percolate.  Add sufficient quantity of menstruum to produce the required volume and then filter. E.g. tincture of belladona, compound tincture of cardamom, strong tincture of ginger. 8/5/2022 Extraction process (HRB)
  • 26. PERCOLATION PROCESS FOR CONCENTRATED PREPARATIONS 26  Used to prepare liquid extracts and solid extracts.  Types of processes are:  Reserve percolation process  Modified percolation process 8/5/2022 Extraction process (HRB)
  • 27. 1. Reserved Percolation Process 27 • In this process, a part of percolate, usually 3/4th of the volume of the finished preparation, is reserved (first percolate) containing high solute concentration. • Percolation process is continued till the drug is completely exhausted. • The percolate thus receives contains traces of active constituents of the drug. • Evaporation or distillation is done to recover the costly menstruum. • Hence, the major portion of the active constituents of the drug are saved from detorioration. • The remaining soft extract is then added to reserve percolate. • Volume make up is done using menstruum. 8/5/2022 Extraction process (HRB)
  • 28. 2. MODIFIED PERCOLATION PROCESS 28 • In percolation process, the drug/percolate (d/p) ratio is about 1:4, the d/p ratio is reduced to 1:3 by modifying the percolation process and hence there is a lot of saving in heat, time and menstruum. • Percolation is the displacement process. • The strong solution of active constituents of drug formed during maceration is displaced by the fresh menstruum when percolation process is started. • Menstruum remaining in contact with the drug dissolves more matter than the flowing menstruum. 8/5/2022 Extraction process (HRB)
  • 29. 29 • Hence, more menstruum is required to exhaust the drug when simple percolation process is used. • In simple percolation process: Drug Imbitition Maceration percolation and collect the percolate, i.e. ¾ of the volume of the finished product. In modified percolation process: Drug-imbibition-maceration-percolation and collect 1000ml of percolate (24hr) -maceration-percolation and collect 1000ml of percolate (12hr) -maceration –percolation and collect 1000ml of percolate (12hr) Drug:percolate 1000gm:3000ml d/p=1:3 8/5/2022 Extraction process (HRB)
  • 30. 30  After exhaustion of the drug, the percolate is evaporated and then mixed with the main percolate.  The final volume is made by adding more of menstruum. 8/5/2022 Extraction process (HRB)
  • 31. Continuous hot percolation process or soxhlet extraction or soxhleation 31  When active constituents of the drug are not freely soluble in the solvent or difficult to be displaced from the cells of the drug, then it becomes necessary to extract the crude drug by action of hot menstruum for a considerable length of time.  The fixed oils from seeds and alkaloids from the drug are extracted by continuous hot percolation process using benzene, chloroform, petroleum, ether etc. Soxhlet apparatus 1. Flask containing the boiling water 2. Soxhlet Extractor: in which the drug to be extracted is packed.  It has a side tube which carries the vapors of the solvent from the flask to the condenser and a siphon tube which siphons over the extract from soxhlet extractor to the flask.  A condenser in which the vapors of the solvent are condensed again into solvent. 8/5/2022 Extraction process (HRB)
  • 33. 33 PROCEDURE  The drug 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  The apparatus is then fitted as shown is figure.  When solvent is boiled on heating flask, it gets converted into vapors.  These vapors enter into the condenser through the side tube and get condensed into hot liquid which falls on column of the drug.  When the extractor gets filled with the solvent, the level of siphon tube also raises up to its top. 8/5/2022 Extraction process (HRB)
  • 34. 34  The solvent containing active constituents in the siphon tube siphon over and run into the flask, thus emptying the body of extractor.  This alteration of filling and emptying the body of extractor goes on continuously until the drug is exhausted (normally 15 times).  The soluble active constituent of the drug remain in the flask where solvent is repeatedly volatilized. 8/5/2022 Extraction process (HRB)
  • 35. Factors affecting the choice of extraction process 35 1. Character of drug Knowledge of pharmacognosy – maceration process if drug is soft, percolation process used when drug is hard and tough 2. Therapeutic value of the drug: when the drug has high therapeutic value, maximum extraction is required, so percolation process is used e.g. Belladona. 3. Cost of drug costly drugs are extracted by percolation process, whereas cheap drugs are extracted by maceration process. 4. Stability of drug: -Thermolabile drugs-maceration or percolation should be done. - No hot extraction process should be carried out. 8/5/2022 Extraction process (HRB)
  • 36. 36 5. solvent:  Maceration process recommended-if water is used as solvent.  Percolation process-nonaqueous solvents. 6. Concentration of product – • The dilute products such as tinctures can be made by using maceration or percolation process, depending on other factors. • For semi-concentrated preparations, such as concentrated infusions, double or triple maceration process can be used. The liquid extracts or dry extracts or dry extracts which are concentrated preparations are prepared by using percolation process. 8/5/2022 Extraction process (HRB)