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EXTRACTION

Extraction is a crucial process in pharmacy for isolating active ingredients from natural sources, involving methods like liquid-liquid, solid-liquid, and Soxhlet extraction. Factors such as solvent choice, temperature, and pH significantly influence extraction efficiency, while various techniques like maceration and percolation are employed to optimize results. The document outlines the principles, processes, and applications of extraction in pharmaceutical contexts, emphasizing the importance of quality control and proper methodology.

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0% found this document useful (0 votes)
39 views86 pages

EXTRACTION

Extraction is a crucial process in pharmacy for isolating active ingredients from natural sources, involving methods like liquid-liquid, solid-liquid, and Soxhlet extraction. Factors such as solvent choice, temperature, and pH significantly influence extraction efficiency, while various techniques like maceration and percolation are employed to optimize results. The document outlines the principles, processes, and applications of extraction in pharmaceutical contexts, emphasizing the importance of quality control and proper methodology.

Uploaded by

Naeem Akhtar
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
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Prepared By

Miss : Marvi
Pharm-D, MBA
Introduction to
Extraction

• Definition: Extraction is
the process of separating
compounds based on their
solubility in different
solvents.
• Importance in Pharmacy:
Used to isolate active
ingredients from natural
sources, purify compounds,
and analyze chemical
composition.
Menstruum:

Liquid used in extraction procedure is


called menstrum.

Terminolonog MARC:The waste material left behind


after extraction is called Marc.
ies
Comminution:

To reduce particle size is called


comminution (increase surface area).
Imbibition:

moist the drug is called imbibition.

Need Of Extraction:

Some gylcosides(sugarcontaning),alkaloids(nitrogen
Contaning),volatile oils(evaporate in air) and resins
are very important to us so we use extraction
process is purify them
Potency can be Controlled.

Deterioration can be controlled.

Advantage Different dosage form can be


s synthesize.

Purify drug has more stability than


unpurified drug.

Adverse drug reactions are less.


Suitable size reduction of crude
drug.(communition,powder)

Select the suitable


liquid/menstruum.

Penetrate the drug into


menstruum.

Supply the heat if needed.

Then filter the Drug.

Press the Marc if needed

Evaporation Technique used to get


purified drug.
Theory Of Extraction

Size reduction: to achieve proper extraction


maximum surface area of contact
But it isnot feasible to reduce the size of material
to cellular level as(it may cause decomposition of
constituents)
V.fine particles may not form good suspension as
they would not sediment at desired rate and
particle size
Principles of
Extraction

• Selective Solubility: Key to successful


extraction; relies on different
solubilities of compounds in solvents.
• Partition Coefficient: Ratio of
solubility in two immiscible solvents,
which predicts how a compound will
distribute.
• Factors Affecting Extraction:
Temperature, pH, solvent polarity, and
particle size.
TYPES OF EXTRACTION

Liquid-Liquid
Extraction
(LLE):
Types of
Separation
Extraction
based on
Techniques
solubility in two
immiscible
liquids.

Supercritical
Fluid
Solid-Liquid
Extraction
Extraction
(SFE): Uses
(SLE):
supercritical CO₂,
Commonly used
beneficial for
for herbal and
thermally
plant extracts.
sensitive
compounds.
(LLE)
Process:
Applications:
Compound
5: Liquid-Liquid Extraction of
partitioning
Extraction (LLE) alkaloids, essential
between aqueous
oils, antibiotics.
and organic layers.

Advantages:
Simplicity and Example
efficiency for Solvents: Water,
water-insoluble ether, chloroform.
compounds.
(SLE)

• : Solid-Liquid Extraction (SLE)


• Process: Solvent penetrates solid
material, dissolving compounds.
• Applications: Common in
obtaining plant extracts (e.g.,
herbal medicines).
• Solvents Used: Ethanol,
methanol, acetone.
• Methods: Maceration, percolation,
and Soxhlet extraction.
Steps in the Extraction Process

Steps in the Extraction Process

Selection of Solvent: Based on target compound's solubility and stability.

Extraction: Mixing solvent with the material.

Filtration: Removing undissolved material.


Concentration and Purification: Often involves evaporation or further
solvent partitioning.
Analysis and Quality Control: Ensuring purity and efficacy of extracted
compounds.
FACTORS

Factors Influencing Extraction Efficiency

Solvent Choice: Must dissolve the desired component but not contaminants.

Temperature: Higher temperatures can increase solubility but may degrade


sensitive compounds.

pH: Affects ionization and solubility, particularly for acidic or basic compounds.

Contact Time: Longer extraction times can increase yield but also extract
impurities.
APPLICATION IN PHARMACY

Drug
Application Developme
s in nt: Isolating
Pharmacy active
and ingredients
Medicine from natural
sources.

Herbal Analytical
Medicines: Testing:
Extraction of Identification
phytochemic of
als for compounds
therapeutic in complex
uses. mixtures.
EXTRACTION
PROCESSES
• Extraction of crude drugs can be done by
various processes depending on physical
nature of drug and chemical properties of
the constituents present in it.
• Various methods used for extraction of
drug include:
• Infusion
• Decoction
• Digestion
• Maceration
• Percolation
Infusion

In this method hot menstruum is poured on


crude drugs for certain period of times

Extraction Decoction
Techniques/proc
ess In this method both drug & menstruum are
boiled together ,for certain period of time

Maceration

In this method drug in powdered form, covered


up in porous cloth and dipped in menstruum for
2-14 days
Digestion

Maceration in the presence gentle heat is called digestion.

Percolation

For this process a column shaped apparatus named


percolator is used

It may be

Open percolator (used for non-volatile liquid)

Fine powder of wet drug is placed in the column & then


add menstruum
The menstruum percolate
time through placed drug.

After appropriate time it is


collected in collector &
water is evaporated to get
pure drug.
• Preparation of the Plant Material
• Select the plant material (e.g., leaves, flowers,
or soft stems) to be used.
• Clean the material to remove dirt and
impurities.
• Dry the material if needed, but fresh material
can also be used.
• Grind or crush the plant material lightly to
increase the surface area for extraction.
• 2. Choosing the Solvent
• Use a suitable solvent, commonly hot or
boiling water for infusions.
• For specific compounds, other solvents like
alcohol or glycerin may be used, but water is
typical in traditional infusion.
• 3. Heating the Solvent
• Heat water until it reaches boiling or the
required temperature.
• Ensure the temperature is appropriate to
avoid degrading sensitive compounds in the
plant material.
• 4. Infusion Process
• Place the prepared plant material in a heat-
resistant container or infusion apparatus.
• Pour the hot water over the plant material to
fully submerge it.
• Cover the container to prevent the loss of
volatile compounds through evaporation.
• 5. Steeping
• Allow the mixture to steep for a specific time, usually 10–30
minutes, depending on the plant material and desired potency.
• For delicate materials like flowers, a shorter steeping time is
sufficient; tougher materials may require longer steeping.
• 6. Filtration
• After steeping, filter the mixture to separate the liquid extract
(infusion) from the solid plant residue.
• Use a fine sieve, muslin cloth, or filter paper to ensure clarity
of the liquid.
• 7. Cooling (Optional)
• Allow the infusion to cool to a safe temperature if it is to be
consumed directly.
• Cooling is optional if the infusion is meant for further
pharmaceutical processing.
• 8. Storage (if applicable)
• If the infusion is not used immediately, store it in an airtight
container to prevent contamination and degradation.
• Refrigerate if the infusion is water-based, as it has a short
shelf life.
• 9. Quality Control
• Check the infusion for clarity, absence of particulate
matter, and desired concentration of active compounds.
• Perform necessary tests for pH, microbial
contamination, or other parameters if require
• 10. Usage or Further Processing
• Use the infusion as it is, or process it further to concentrate
the extract, mix with other formulations, or stabilize it.
• This process ensures the effective extraction of heat-stable
and water-soluble compounds while preserving the active
constituents.
• Maceration is a widely used extraction
method in pharmaceutics for isolating
bioactive compounds from plant materials. It
involves soaking plant materials in a solvent
to allow the soluble constituents to dissolve.
The method can be classified into single,
double, and triple maceration based on the
number of extractions performed. Below are
the step-by-step processes for each type:
• 1. Single Maceration
• This is the simplest form of maceration, where the plant
material undergoes extraction once.
• Steps:
1.Preparation of Plant Material:
1.Crush or grind the plant material into small pieces to
increase the surface area.
2.Dry the material if necessary to remove moisture.
2.Selection of Solvent:
1.Choose an appropriate solvent (e.g., ethanol, water, or a
mixture) based on the nature of the active compound.
3.Soaking:
1.Place the plant material in a container.
2.Add the solvent in a specified ratio (e.g., 1:10 w/v for
plant material to solvent).
4)Maceration:
•Leave the container sealed and let it stand for a
specified duration (e.g., 24-48 hours) at room
temperature or with gentle heating (if heat-stable).
•Stir occasionally to enhance extraction.
•5)Filtration:
•Filter the mixture through muslin cloth or filter paper
to separate the liquid extract from the residue.
•6)Concentration (Optional):
•Concentrate the extract under reduced pressure if
needed to obtain the desired concentration.
• 2. Double Maceration
• In this method, the plant material is macerated
twice with fresh solvent, increasing the yield of
active constituents.
• Steps:
1.Follow the steps from Single Maceration
(Steps 1-5) to obtain the first extract.
2.Residue Re-soaking:
1.Take the solid residue left after the first
maceration.
2.Add fresh solvent (usually half the volume
used in the first maceration).
•3)Second Maceration:
•Repeat the soaking and standing process for another 24-
48 hours.
•4)Filtration:
•Filter the second extract as before.
•5)Combination of Extracts:
•Mix the first and second extracts to ensure uniformity.
•6)Concentration (Optional):
•Concentrate the combined extract under reduced
pressure if needed
• 3. Triple Maceration
• This method involves three rounds of maceration for
maximum extraction efficiency.
• Steps:
1.Follow the steps from Single Maceration (Steps 1-5) to
obtain the first extract.
2.Second Maceration:
1.Use the residue from the first maceration.
2.Add fresh solvent and repeat the process as in Double
Maceration.
3.Filter to obtain the second extract.
1.Third Maceration:
1.Use the residue from the second
maceration.
2.Add fresh solvent for the third round.
3.Repeat the soaking, maceration, and
filtration processes.
2.Combination of Extracts:
1.Mix all three extracts obtained from the
successive macerations.
3.Concentration (Optional):
1.Concentrate the combined extract under
reduced pressure.
• General Considerations:
• Duration: The soaking time for each
maceration step can vary depending on the
solubility of the target compounds.
• Temperature: Keep the temperature
appropriate for the solvent and compound to
prevent degradation.
• Solvent Ratio: Ensure the solvent quantity is
sufficient to cover the plant material
completely.
• Quality Control: Evaluate the extract using
standardization techniques to ensure
• Advantages:
• Simple and cost-effective.
• Suitable for heat-sensitive compounds (since no high
temperatures are involved).
• Double and triple maceration methods improve
extraction yield and efficiency.
• Disadvantages:
• Time-consuming.
• Requires large quantities of solvent, which can increase
costs.
• Inefficient compared to advanced methods like
percolation or Soxhlet extraction.
• The percolation method is a widely used
extraction process in pharmaceutics to obtain
active constituents from plant or herbal
materials. It is particularly employed to
prepare tinctures, extracts, and other liquid
pharmaceutical preparations. Below is a step-
by-step breakdown of the method and
process
• Step-by-Step Percolation Process
• 1. Preparation of the Drug Material
• Selection: Choose the plant or herbal material (drug) to
be extracted.
• Size Reduction: Reduce the size of the material (e.g.,
to coarse or moderately fine powder) to increase the
surface area for extraction.
• Screening: Pass the material through a sieve of
appropriate mesh size to ensure uniformity.
• Moistening: Moisten the powdered material with the
solvent (menstruum) and allow it to stand for a specific
period (this is called maceration or conditioning). This
step helps in swelling the drug and improves the
penetration of the solvent during percolation.
• 2. Packing the Percolator
• A percolator is a cylindrical vessel used for
the process.
• The moistened drug material is uniformly
packed into the percolator to avoid channels or
void spaces, which could affect the extraction
efficiency.
• A filter material (e.g., cotton, muslin cloth) is
placed at the bottom of the percolator to
prevent drug particles from clogging the
outlet.
• 3. Adding the Solvent (Menstruum)
• The solvent (e.g., water, alcohol, or a
combination) is poured onto the packed drug
material in the percolator.
• Allow the solvent to completely saturate the
material and start dripping through the outlet
at the bottom
• 5. Continuous Extraction
• Continue adding solvent at the top to replace
the percolate collected at the bottom.
• Ensure the solvent passes through the entire
column of drug material, extracting the active
components efficiently.
• 6. Collection of Percolate
• The percolate (liquid extract) is collected in
fractions.
• Initial fractions, known as "strong percolates,"
contain the highest concentration of active
constituents.
• Subsequent fractions may have lower
concentrations and can be combined or
processed further, depending on the desired
potency of the extract
• 7. Final Processing
• Combine the collected percolate fractions, if
needed, and concentrate them by evaporation
(optional) to achieve the desired strength.
• If required, filter the extract to remove any
particulate matter.
• Standardize the preparation according to
pharmaceutical guidelines (e.g., by adjusting
the volume or concentration).
• Key POINTS
1.Choice of Solvent:
1.The type of solvent depends on the solubility of the active
constituents. Common solvents include alcohol, water, or
mixtures of both.
2.Solvent Ratio:
1.Ensure an optimal solvent-to-drug ratio for efficient
extraction without excessive waste.
3.Avoiding Channeling:
1.Proper packing and saturation of the drug material are
critical to avoid channeling, which reduces extraction
efficiency.
4.Filtration:
1.Use appropriate filtration techniques to ensure the final
product is free of contaminants.
• Applications in Pharmaceutics
• Preparation of herbal tinctures and liquid
extracts.
• Extraction of alkaloids, glycosides, tannins,
and other phytoconstituents.
• Used in pharmaceutical industries for
producing concentrated liquid extracts for
further formulation into tablets, capsules, or
syrups.
• By following these steps, the percolation
method ensures efficient extraction of active
ingredients for pharmaceutical applications.
• The soxhlet extraction method is a
widely used technique in pharmaceutics
and other scientific fields to extract
bioactive compounds from plant
materials or other solid substances using
a solvent. Here’s a step-by-step guide to
the Soxhlet extraction process:
• Materials Needed:
1.Soxhlet apparatus (comprising a round-bottom
flask, extraction chamber, and condenser).
2.Solvent (e.g., ethanol, methanol, hexane,
water, etc., depending on the compound being
extracted).
3.Sample material (e.g., plant powder).
4.Heat source (e.g., heating mantle or water
bath)
• Process Steps:
• 1. Preparation of the Sample:
• Dry the sample (e.g., plant material) to remove
moisture that could interfere with the
extraction process.
• Grind the material into a fine powder to
increase the surface area for extraction.
• 2. Selection of Solvent:
• Choose an appropriate solvent based on the
polarity of the target compound. For instance:
• Non-polar solvents (e.g., hexane) are used
for non-polar compounds (e.g., oils, lipids).
• Polar solvents (e.g., ethanol) are used for
polar compounds (e.g., alkaloids,
flavonoids).
• 3. Assembling the Soxhlet Apparatus:
• Place the ground sample into a thimble made
of filter paper or fabric and insert it into the
Soxhlet extractor.
• Fill the round-bottom flask with the selected
solvent.
• Connect the Soxhlet extractor and the
condenser on top.
• Ensure all connections are tight to avoid
solvent loss.
• 4. Heating:
• Heat the solvent in the round-bottom flask gently using a
heating mantle or water bath.
• The solvent vaporizes and travels up into the condenser,
where it cools and condenses back into liquid form
• 5. Extraction Process:
• The condensed solvent drips onto the sample material in
the thimble, extracting the desired compounds.
• The solvent, now containing dissolved compounds, siphons
back into the flask.
• This process repeats automatically, ensuring continuous
extraction.
• 6. Monitoring and Timing:
• Allow the extraction to proceed for several
cycles (typically 4–12 hours, depending on the
material and solvent).
• Monitor the system to ensure no leaks or
overheating occur
• 7. Completion of Extraction:
• Once the solvent in the siphon appears
colorless or shows no further change, the
extraction is considered complete.
• 8. Recovery of the Extract:
• Remove the solvent from the extract using a
rotary evaporator or distillation to obtain a
concentrated extract.
• The remaining solid material in the thimble is
discarded.
• 9. Post-Extraction Processing:
• Purify the extract if needed (e.g., by filtration,
centrifugation, or column chromatography).
• Dry the extract under vacuum or freeze-drying
for further analysis or formulation.
Advsantages and Limitations of
Extraction Techniques

Advantages: Selective compound isolation,


scalable, adaptable to various substances.
Limitations: Solvent toxicity, extraction yield
variability, need for post-extraction
purification.
Liquid-Liquid Extraction
• Definition
• The process in which a solute distribute
itself b/w two solvent and these two
solvent are immesible (we not soluble)
to each other and this method…
• Conditions:
• Temperature, Pressure are kept
constant during this process.
• The solvent(Aquous solvent and non-
Aquous solvent are immiscible to each
other.
• The solvent ratio have small polarity
difference.
• Base
• Solvent Extraction is based on
distribution law.
• Ether extraction in an example of
solvent extraction
Distribution Law
• This law is given by Nernst(1864-1906)
• Statement: A solute distribute itself B/W two immiscibile
solvent with a constant ratio of concentration
irrespective the amount of solute ‘added’
• Other names of Distribution law
• Partition law
• Nernst distribution law
• Nernst partition
Experimental Verification
• Take a beaker add water and Add KI salt and the salt
ionize as
• KI K+I
• Now Add I.I react with I and formed I
• I+I I
• Add ccl4 in the beaker & ccl4 &water
are immisible each other
• I+ I I
con:
• I is removed toward organic layer & purple colors
dominate.Brown color of I is fade out.
• A Equilibrium is established & no color change occur at
equilibrium.

• Formula
• K=[C]organic layer/[C]Aquous layer
• K=Vo/Va
Distribution Law

• Dependence:
• Temperature and pressure:
•A B
• K=[ B]/[A] concentration of product
• Distribution law depend on temperature as well as pressure.
Distribution is only applicable at equllibrium.Equllibrium is
the property of reversible process.
• The effect of temperature & pressure in reversible process is
explain by le-chattier. For Distribution law temperature and
pressure would be constant.
• Dilute concentration:
• This law is only applicable for dilute
solution .
• Those solution in which amount of solute is
less .
• Same Molecular state:
• The state of solute be same the molecule
should not be polymerization.
• Equilibrium Concentration:
• Distribution law is only applicable at
the state of equilibrium.
• Any system require some time to attain
equilibrium.
• NON Missibility of Solvent
• Solvent should not disolved to each other
• The two solvent ( aqeous solvent & organic
solvent should not dissolved or react to each
other)
• Normally we used are polar solvent(water) &
other is non-polar solvent)
• POLAR: water, methanol,ethanol)
• NON-POLAR SOLVENT: Ether,Petrol,ccl4
• Distribution coefficient:
• Actually a ratio b/w the concentrationof solute in
organic layer & concentration of solute in aqeous layer
• It is also known as partition coefficient.
• representation:kd
• Formula
• Kd=
• Suppose
• We have a solute “A”

(KD)A = [A]org/
[A]aq
Distribution Ratio
• Tell us how much solute is moved from one solvent toanother.
• Ratio B/W the amount(conc:) of solutes in aqeous layer.
• Formula

• D=CA/CA

• D=Distribution ratio
• A=all types of solute
• C=Concentration represents
• If distribution ratio is 100 increase better separation
• If A is less than in separation
• Distribution is less than 1 less separation.
Liquid-Liquid Extraction
• Types of Extraction
1)Batch Extraction
2)Continous Extraction
3)Counter current Extraction
4)Multiple Extraction

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