Extraction involves the separation of medicinally active portions of plant or animal tissues from the inactive or inert components by using selective solvents by standard extraction procedures.
Extraction methods include solvent extraction, distillation method, pressing and sublimation according to the extraction principle. Solvent extraction is the most widely used method.
The extraction of natural products progresses through the following stages:
- (1) the solvent penetrates into the solid matrix;
- (2) the solute dissolves in the solvents;
- (3) the solute is diffused out of the solid matrix;
- (4) the extracted solutes are collected.
Efficiency of extraction depends upon following factors
- The properties of the extraction solvent,
- The particle size of the raw materials,
- The solvent-to-solid ration,
- The extraction temperature &
- The extraction duration
Note: Expression is the physical act of applying pressure to squeeze out oils or juices from plants. This was normally achieved with a tincture press.
Menstruum:
The solvent used for extraction is known as a menstruum
Marc
Inert insoluble material that remains after extraction
Galenical:
All preparations that are prepared by using one of the various extraction processes is known as Galenicals.
The products obtained from plants are relatively impure liquids, semisolids, or powders intended only for oral or external use. These include classes of preparations known as decoctions, infusions, fluidextracts, tinctures, pilular (semisolid) extracts, and powdered extracts. Such preparations have been called galenicals.
Steps Involved in the Extraction of Medicinal Plants
In order to extract medicinal ingredients from plant material, the following sequential steps are involved-
- Size reduction
- Extraction
- Filtration
- Concentration
- Drying
Solvent/menstruum used in extraction process
1. Water
-It is polar solvent and is used in the extraction of a wide range of polar compounds.
-Solvent for protein, coloring matter, gums, glycoside, sugar, alkaloid salts, enzymes and many organic acid and salts.
-Wax, fat, fixed oil and most alkyl halides are insoluble in water.
-it is cheap, nontoxic, nonflammable, and highly polar.
Disadvantage:
-Wide solvent action-dissolve a wide range of substances that are undesirable
-The growth of molds and bacteria-need of preservatives
-Hydrolysis of drug
-Required large amount of heat to obtain aqueous concentrate preparation than non-aqueous
-Fermentation may occur-so degradation of the product
2.Alcohol
– It is also polar in nature, miscible with water, and could extract polar secondary metabolites.
-Solvent for alkaloids, alkaloids salt, glycoside, volatile oils and resins.
-Also dissolve coloring matter, tennis and organic acids and salts
-Does not dissolve albuminous matters, gums, wax, fat, fixed oil and sugar
Advantage
-No mold and bacterial growth if the concentrate is 20% or above 20% (self-preservative).
-Required small amount of heat to get concentrate preparation.
-Dissolve selective active constituent of drug.
-Neutral solvent.
Disadvantage: it is costly & flammable and volatile
Other Solvents Used for Extraction
3. Chloroform
- Nonpolar solvent
- Useful in the extraction of compounds such as terpenoids, flavonoids, fats, and oils.
Advantages-
- Colorless, sweet smell, and is soluble in alcohols.
- Also absorbed and metabolized in the body
Disadvantages– sedative and carcinogenic property.
4. Ether
- Nonpolar solvent
- Useful in the extraction of compounds such as alkaloids, terpenoids, coumarins, and fatty acids.
Advantages
- Miscible with water.
- Has low boiling point.
- tasteless in nature.
Disadvantages- highly volatile and flammable in nature.
5. Ionic liquid (green solvent)
- It is highly polar and extremely heat stable (remain in a liquid state even at 3,000.
- It is Miscibility with water and other solvent.
Advantages-
- Excellent solvent that attracts and transmit microwave
- It is nonflammable
Various type of Methods of Extraction
1. Infusion method
Drug is placed at bottom of the pot + add water/hot water and stirred three to four times, stands a usually 15 minutes. After 15 minutes, filtering off the liquid without pressing the marc.
or
Drug is Enclosed in muslin bag& suspended in the water/hot water in a pot. stirring is not required due to slow circulation.
Fresh Infusion
- Coarse powder of drug + water (aqueous solution/menstruum)
- Used within 12 hours after its preparation otherwise infusion get spoilt due to fungal and bacterial growth.
- Example: fresh infusion of
Concentrated infusion
- Prepared by double/triple maceration process
- 8 x stronger than fresh infusion
- Alcohol(20-25% in concentration) used as solvent
- Alcohol-can be stored for a longer period of time
- Eg. Conc. infusion of Quassia, Conc. infusion of chirata
2. Decoction
- 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, heat-stable constituents from hard & woody materials.
- 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.
- This process is typically used in preparation of Ayurvedic extracts called “quath” or “kawath”.
3. Maceration
- In this process, the whole or coarsely powdered crude drug is placed in a stoppered container. Then the mesntruum is poured on top until completely covered the drug material. The container is then closed & allowed to stand at room temperature for a period of at least 3 days with frequent agitation until the soluble matter has dissolved. The mixture then is strained, the marc (the damp solid material) is pressed, and the combined liquids are clarified by filtration or decantation after standing.
- This method is convenient and very suitable for thermolabile plant material.
Note: Plant material in fine powder form is never used, as it makes subsequent clarification/filtration of the extract difficult.
Process of extraction works by molecular diffusion, which is very slow. Occasional shaking assists diffusion and also ensures dispersal of the concentrated solution accumulating around the surface of the particles, thereby bringing fresh menstruum to the particle surface for further extraction.
A closed vessel is used to prevent evaporation of the menstruum during the extraction period and thus avoids batch to batch variation.
Maceration Process for Organized and Unorganized Crude Drugs
- Organized drugs have a defined cellular structure whereas unorganized drugs are non-cellular.
- Bark and roots are examples of organized crude drugs, while gum and resin are unorganized crude drugs.
Organized Drug/simple maceration
- Placed crude Organized drug in closed vessel & fill with entire volume of menstruum.
- Shake occasionally for 7 days
- Strain liquid, press the marc.
- Both expressed liquid & strained liquid are mixed & finally preparation is filtered to remove insoluble cell content & stored. Filtrate is not adjusted for volume.
- Example: Tincture of orange(IP), Tincture of lemon, tincture of capsicum (BPC), compound tincture of gentian, tincture of lemon, and tincture of squill (BPC).
Note: During maceration of organized drugs, the marc is pressed because a considerable proportion of liquid adheres to it and cannot otherwise be separated. Also volume is not adjusted because a variable amount of liquid containing soluble matter is left in the marc. If the volume is adjusted, a weak product will result.
Unorganized Drug/modified maceration
- Drug + four-fifths (4/5) of menstruum (in most cases)
- Shake occasionally on days 2 to 7, as specified.
- Decant the liquid. Marc is not pressed.
- Filter the liquid and add remaining menstruum (1/5 part) through the filter to adjust the final volume.
- Example: Tincture of the tolu, Compound tincture of benzoin, tincture of myrrh (BPC).
Note: In maceration of unorganized drugs, the marc is not pressed because the desirable material is mostly dissolved and the remaining marc is gummy and slimy. Thus, it is neither practicable nor necessary to press it. or Unorganised drug behave like simple chemical (sugar) and dissolve very easily and quickly.(so need not to press the marc).
4. Percolation
Percolation is used mostly to prepare tincture & fluid extract. It is also known as Exhaustive Extraction.
A percolator (a narrow, cone shaped vessel open at both ends) is used to extract active ingredients from the crude drugs.
Various types of Percolation
a) Simple percolation
b) Percolation process for concentrate preparation
c) Continuous hot percolation/Soxhlet
Steps involved in percolation process:
I. Size Reduction
Size reduction increases the surface area of the crude drug and more surface area of the crude drug will be available to react with the menstruum to insure complete exhaustion of the crude drug. Size reduction is also helpful for uniform packing of the crude drug in a percolator and reducing the moment of menstruum in the percolator.
II. Imbibition
In the Imbibition step, the powdered crude drug is moistened with menstruum in well closed container for 4 hrs to swell and to escape entrapped air. During imbibition step, the menstruum penetrates the cell wall. This initial moistening of the crude drug powder is very important because it reduces the chances of choking of percolator though the dried drug swells when comes into contact with menstruum. Imbibitions also prevent the washing of fine particles of the crude drug during percolation.
.III. Packing
Moistened drug is packed in percolator & additional menstruum is added to form shallow layer.
The lower end of the percolator should be plucked with cotton and then place the drug powder layer by layer. Two third of the percolator should be covered with the drug on which place the piece of filter paper and wash sand should be placed on the top of the filter paper. This prevents any type of disturbance of the crude drug by the flow of menstruum.
IV. Maceration
V. Percolation
VI. Pressing the marc
5. Hot Continuous Extraction (Soxhlet)
The Soxhlet extraction is an automatic continuous extraction method with high extraction efficiency that requires less time and solvent consumption than maceration or percolation.
Principle: Soxhlet utilizes the principle of reflux and siphoning to continuously extract the herb with fresh solvent.
Soxhlet extraction method is suitable when
- Menstruum has less penetration into the cellular tissue.
- Active constituents are not readily extracted with a solvent.
Note: The high temperature and long extraction time in the Soxhlet extraction will increase the possibilities of thermal degradation.
Fixed oil from seed, alkaloid from drug are extract by soxhlet extraction process using Benzene, chloroform and petroleum, Ether etc.
Apparatus-
The apparatus consist of three important parts:
- A . Flask (round bottom) containing the boiling solvent.
- B . Soxhlet Extractor in which the drug to be extracted is packed.It has a side tube which carries the vapours of the solvent from the flask to the condenser and a syphon tube which syphons over the extract from soxhlet extractor to the flask.
- C . A condenser in which the vapours of the solvent are condensed again into solvent
Procedure:-
- Placed finely ground crude drug which is packed into a porous bag/thimbe (made of filter paper) in a soxlet extractor..
- The solvent is placed in the flask. & extracting solvent is boiled. It gets converted into vapours. & vapour is condensed in reflux condensor.
- When solvent is boiled on heating the flask,it gets converted into vapours.These vapours enter into the condenser through the side tube and get condensed into hot liquid which falls on the column of the drug.When the extractor gets filled with the solvent ,the level of syphon tube also raise up to its top.The solvent containing active constituents of the drug in the syphon tube syphon over and run into the flask ,thus emptying the body of extractor .This alternation of filling and emptying the body of extractor goes on continuously. The soluble active constituents of the drug remain in the flask while the solvent is repeatedly volatilised. The process of filling and emptying of the extractor is repeated until the drug is exhausted. Normally the process is repeated about 15 times for complete exhaustion of the drug.
Advantage:
- Large amount of drug can be extracted with much smaller quantity of solvent(fewer solvents).
- Tremendous economy in terms of time, energy & ultimately financial inputs.
- Small scale used a batch-process.
- Becomes more economical when converted into continuous extraction.
Demerits:
Thermolabile drugs and constituents are not suitably extracted by this method.
6. Digestion
- Drug is extracted by heating at a particular pressure. This will increase the penetration power of the menstruum so that there is complete extraction of the drug.
- Digestor: Metal vessel
7. Counter-current Extraction
In counter-current extraction (CCE), wet raw material is pulverized using toothed disc disintegrators to produce a fi ne slurry. In this process, the material to be extracted is moved in one direction (generally in the form of a fi ne slurry) within a cylindrical extractor where it comes in contact with extraction solvent. The further the starting material moves, the more concentrated the extract becomes. Complete extraction is thus possible when the quantities of solvent and material and their flow rates are optimized. The process is highly efficient, requiring little time and posing no risk from high temperature. Finally, sufficiently concentrated extract comes out at one end of the extractor while the marc (practically free of visible solvent) falls out from the other end.
7. Ultrasound Extraction (Sonication)
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. Although the process is useful in some cases, like extraction of rauwolfi a root.
Its large-scale application is limited due to the higher costs.
One disadvantage of the procedure is the occasional but known deleterious effect of ultrasound energy (more than 20 kHz) on the active constituents of medicinal plants through formation of free radicals and consequently undesirable changes in the drug molecules
8. Supercritical Fluid Extraction
The different component in the supercritical fluid extraction is the first one is a fluid reservoir which contains the fluid-like gas cylinder in the case of CO2. Another one is the pump; the pump may be a syringe pump or reciprocating pump. Another important is the extractor which may be made of stainless steel and can with a stand to high pressure like 300 to 600 atmosphere. Another important component of the supercritical fluid extractor is the restrictor. It is important for the controlled and systematic release of the pressure inside the extractor vesicle. The restrictor may be a fixed type or variable type. The isolated constituent is collected in a collector where it can be detected with the help of a detector. Sometimes modifiers are also added into the supercritical fluid to increase its versatility like one to ten percent of methanol is added in CO2.
9. Hydrodistillation
It is method popular methods to separate the essential oil from crude drugs.
In order to isolate essential oils by hydrodistillation, the aromatic plant material is packed in a still and a sufficient quantity of water is added and brought to a boil; alternatively, live steam is injected into the plant charge. Due to the influence of hot water and steam, the essential oil is freed from the oil glands in the plant tissue. The vapor mixture of water and oil is condensed by indirect cooling with water. From the condenser, distillate flows into a separator, where oil separates automatically from the distillate water.
Three are three types of hydrodistillation for isolating essential oils from plant materials:
- Water distillation
- Water and steam distillation
- Direct steam distillation
A brief summary of various extraction methods
| Method | Solvent | Temperature | Pressure | Time | Volume of organic solvent consumed | Polarity of natural products extracted |
|---|---|---|---|---|---|---|
| Maceration | Water, aqueous and non-aqueous solvents | Room temperature | Atmospheric | Long | Large | Dependent on extracting solvent |
| Percolation | Water, aqueous and non-aqueous solvents | Room temperature, occasionally under heat | Atmospheric | Long | Large | Dependent on extracting solvent |
| Decoction | Water | Under heat | Atmospheric | Moderate | None | Polar compounds |
| Reflux extraction | Aqueous and non-aqueous solvents | Under heat | Atmospheric | Moderate | Moderate | Dependent on extracting solvent |
| Soxhlet extraction | Organic solvents | Under heat | Atmospheric | Long | Moderate | Dependent on extracting solvent |
| Pressurized liquid extraction | Water, aqueous and non-aqueous solvents | Under heat | High | Short | Small | Dependent on extracting solvent |
| Supercritical fluid extraction | Supercritical fluid (usually S-CO2), sometimes with modifier | Near room temperature | High | Short | None or small | Nonpolar to moderate polar compounds |
| Ultrasound assisted extraction | Water, aqueous and non-aqueous solvents | Room temperature, or under heat | Atmospheric | Short | Moderate | Dependent on extracting solvent |
| Microwave assisted extraction | Water, aqueous and non-aqueous solvents | Room temperature | Atmospheric | Short | None or moderate | Dependent on extracting solvent |
| Pulsed electric field extraction | Water, aqueous and non-aqueous solvents | Room temperature, or under heat | Atmospheric | Short | Moderate | Dependent on extracting solvent |
| Enzyme assisted extraction | Water, aqueous and non-aqueous solvents | Room temperature, or heated after enzyme treatment | Atmospheric | Moderate | Moderate | Dependent on extracting solvent |
| Hydro distillation and steam distillation | Water | Under heat | Atmospheric | Long | None | Essential oil (usually non-polar) |
MCQ Quiz
1. Which extraction method involves soaking crushed plant material in a solvent for several days?
a) Percolation
b) Maceration
c) Infusion
d) Decoction
Answer: b) Maceration
2. Soxhlet extraction is mainly used for:
a) Water-soluble compounds
b) Continuous solvent extraction
c) Steam distillation
d) Cold maceration
Answer: b) Continuous solvent extraction
3. What is the purpose of using solvents in extraction?
a) To boil the extract
b) To dissolve bioactive compounds
c) To evaporate water
d) To preserve the drug
Answer: b) To dissolve bioactive compounds
4. Which solvent is commonly used for extracting flavonoids?
a) Water
b) Ethanol
c) Benzene
d) Acetone
Answer: b) Ethanol
5. Which method uses water or steam to extract essential oils?
a) Maceration
b) Percolation
c) Steam distillation
d) Soxhlet extraction
Answer: c) Steam distillation
6. What is percolation in pharmaceutics extraction?
a) Heating the extract
b) Continuous flow of fresh solvent through drug material
c) Soaking in solvent without agitation
d) Evaporation of solvent
Answer: b) Continuous flow of fresh solvent through drug material
7. Which extraction method is suitable for heat-sensitive compounds?
a) Soxhlet extraction
b) Decoction
c) Cold maceration
d) Infusion
Answer: c) Cold maceration
8. Which modern extraction technique uses microwave energy to speed up extraction?
a) Percolation
b) Soxhlet extraction
c) Microwave-assisted extraction
d) Maceration
Answer: c) Microwave-assisted extraction
9. Supercritical fluid extraction mainly uses which substance?
a) Ethanol
b) Water
c) Carbon dioxide (CO₂)
d) Acetone
Answer: c) Carbon dioxide (CO₂)
10. Which factor increases the rate of extraction?
a) Larger particle size
b) Decreased temperature
c) Increased surface area
d) Reduced solvent contact
Answer: c) Increased surface area
11. The residue left after extraction of plant material is called:
a) Extract
b) Marc
c) Menstruum
d) Solution
Answer: b) Marc
12. Which of the following involves continuous solvent extraction with circulation?
a) Maceration
b) Percolation
c) Soxhlet extraction
d) Decoction
Answer: c) Soxhlet extraction
13. Which type of solvent is preferred for extracting alkaloids?
a) Acidic solvents
b) Basic solvents
c) Neutral solvents
d) Water only
Answer: a) Acidic solvents
14. Which extraction method is best for large-scale industrial use?
a) Maceration
b) Percolation
c) Infusion
d) Decoction
Answer: b) Percolation
15. What does the term “menstruum” refer to in extraction?
a) Solid residue
b) Solvent used in extraction
c) Extracted drug
d) Filtrate
Answer: b) Solvent used in extraction
16. Which method involves boiling plant material with water to extract active constituents?
a) Infusion
b) Decoction
c) Maceration
d) Percolation
Answer: b) Decoction
17. Which extraction method is based on the solubility difference in two immiscible liquids?
a) Chromatography
b) Solvent extraction (liquid-liquid extraction)
c) Filtration
d) Evaporation
Answer: b) Solvent extraction (liquid-liquid extraction)
18. What does the term “extract” mean in pharmaceutics?
a) The solvent used
b) Residue left behind
c) Concentrated solution obtained after extraction
d) Raw drug material
Answer: c) Concentrated solution obtained after extraction
19. Which method uses cold solvent soaking at room temperature?
a) Decoction
b) Cold maceration
c) Percolation
d) Soxhlet extraction
Answer: b) Cold maceration
20. Which is a disadvantage of Soxhlet extraction?
a) Very fast process
b) Not effective for heat-sensitive compounds
c) Requires no solvent
d) Uses cold solvents only
Answer: b) Not effective for heat-sensitive compounds
FAQs
1. What is extraction in pharmaceutics?
Extraction is the process of separating active constituents or bioactive compounds from raw plant or animal materials using a suitable solvent called menstruum. It is essential for obtaining purified drugs and their formulations.
2. What are the common methods of extraction used in pharmaceutics?
Common methods include maceration, percolation, decoction, infusion, digestion, Soxhlet extraction, microwave-assisted extraction, ultrasonic extraction, and supercritical fluid extraction.
3. How does Soxhlet extraction work?
Soxhlet extraction continuously extracts a compound by repeatedly washing the solid material with fresh hot solvent through reflux and siphoning, which improves extraction efficiency of compounds with limited solubility.
4. What is the difference between maceration and percolation?
Maceration involves soaking the drug material in solvent for a prolonged time, while percolation involves the continuous passage of solvent through a packed bed of drug material for faster and more complete extraction.
5. Which extraction method is preferred for heat-sensitive compounds?
Cold maceration or extraction methods that do not involve heat, such as ultrasonic extraction or supercritical fluid extraction, are preferred to avoid degradation of heat-sensitive constituents.
6. What factors affect the efficiency of extraction?
Factors include the nature of the drug, particle size, solvent type, temperature, pH, and duration of solvent contact with the material.
7. What is supercritical fluid extraction?
Supercritical fluid extraction uses supercritical CO₂ as a solvent at high pressure and temperature to extract compounds efficiently without thermal degradation, widely used for heat-sensitive and high-value extracts.
8. Why is solvent choice important in extraction?
The solvent must selectively dissolve the target compounds, be compatible with the drug material, and ideally be non-toxic, easy to remove, and inexpensive. Different solvents target different classes of compounds like alkaloids, flavonoids, oils, etc.
9. Can extraction be used for large-scale industrial production?
Yes, methods like percolation and Soxhlet extraction are scalable and are used at industrial levels to produce herbal extracts, essential oils, and active pharmaceutical ingredients.
10. What are the disadvantages of Soxhlet extraction?
It is time-consuming, uses large amounts of solvent and heat, which may degrade heat-sensitive compounds, making it less suitable for some extracts.