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Microwave-Assisted
Extraction Techniques
for Herbal Drugs
Anurag Kumar
12421EN001
2nd November, 2015
Contents
 Introduction
 Microwave theory
 Extraction principle
 Instruments
 Closed vessel
 Open vessel
 Application of MAE
 Factors affecting MAE
 Conclusion
INTRODUCTION
 Microwave-assisted extraction is an efficient method which
involves deriving natural compounds from raw plants.
 Microwave extraction allows organic compounds to be extracted
more rapidly, with similar or better yield as compared to
conventional extraction methods.
 MAE of anthraquinone in pure alcohol at 60°C for 30 minutes
gives a recovery of 65% which results from 3 days maceration in
pure ethanol at room temperature.
 The advantages that MAE has over other techniques such as
Soxhlet are:
 Reduction in extraction time
 Improved yield
 Better accuracy
 Suitable for thermolabile substances
INTRODUCTION
INTRODUCTION
MICROWAVE THEORY
 Microwaves are non-ionizing electromagnetic waves of
frequency between 300MHz to 300 GHz and positioned between
the X-ray and infrared rays in the electromagnetic spectrum.
 Microwaves serves two major purposes:
 Communication
 Energy vectors
 The energy vector application is the direct action of waves on
materials that has the ability to convert a part of the absorbed
electromagnetic energy to heat energy.
 As any other EM wave we have two parts of Microwaves
 Electric field
 Magnetic field
MICROWAVE THEORY
 In MAE, heating occurs in a targeted and selective manner with
practically no heat being lost to the environment as the heating
occurs in a closed system.
 This unique heating mechanism significantly reduces the
extraction time (usually less than 30min) as compared to
Soxhlet.
MICROWAVE THEORY
EXTRACTION PRINCIPLE
 Dried plants contain a minute microscopic trace of moisture
which serves as target for microwave heating.
 High temperature and pressure is generated inside the oven.
 High temperature causes dehydration of cellulose which
accounts for its reduction of mechanical strength.
 The MAE process is as follows:
 Microwave radiation
 Moisture get heated up
 Moisture evaporates
 Generation of tremendous pressure on cell wall
 Swelling of plant cell
 Rupture of the cell
 Leaching out of phyto-constituents
 This phenomenon can be intensified if the plant matrix is
impregnated with solvents with higher heating efficiency under
microwave.
EXTRACTION PRINCIPLE
INSTRUMENTS
 There are two types of commercially available MAE systems:
 Closed extraction vessels
 Focused microwave ovens
 The former performs extraction under controlled pressure and
temperature.
 In the latter, only a part of the extraction vessel containing the
sample is irradiated with microwave.
Open and Closed-vessel system
INSTRUMENTS
 Both systems are available as multi-mode and single-mode.
 A multi-mode system allows evenly radiation of sample by
random dispersion of microwaves.
 Single-mode (aka focused system) allows focused radiation on a
restricted zone by a much stronger electric field.
INSTRUMENTS
 Both multi-mode and focused system comprises of the following
four components:
 Microwave generator: magnetron which generates
microwave energy
 Wave guide: propagates microwave to microwave cavity
 The applicator: where the sample is placed
 Circulator : allow microwave to move in forward direction
CLOSED VESSEL
 With closed vessel extraction, pressurised microwave assisted
extraction is performed under pressure (with or without
regulation).
 The pressure allows temperatures above boiling points of the
solvents to be reached enhancing speed and efficiency.
 To avoid overpressure, power, temperature and pressure can be
controlled.
 When dealing with thermolabile compounds, high temperature
causes degradation of analytes. Therefore, the open system is
chosen.
Advantages of closed-vessel system
 Decreased in extraction time
 Loss of volatile substances is avoided
 Less solvent is required because no evaporation occurs
 No hazardous fumes during acid microwave since it is a
closed vessel
Disadvantages of closed-vessel system
 High pressure used poses safety risks
 The usual constituent material of the vessel does not allow high
solution temperatures
 Addition of reagents is impossible since it is a single step procedure
 Vessel must be cooled down before it can be opened to prevent loss of
volatile constituents.
OPEN VESSEL
 Extraction is made at atmospheric pressure.
 The maximum possible temperature is determined by the boiling point of
the solvent at that pressure.
 Loss of vapours is prevented by the presence of a cooling system on the
top of the extraction vessel that causes condensation of solvent vapours.
 Heating is homogenous and efficient.
Advantages of open-vessel system
 Increased safety
 Addition of reagent is possible
 Vessels made of various material can be used
 Excess solvent can be removed easily
 Ability to process large samples
 No requirement for cooling down or depressurisation
 Low cost of equipment
 Suitable for thermolabile products
Disadvantages of open-vessel system
 This method is less precise than in close-vessel system
 The sample throughput is lower as open system cannot process
many samples simultaneously
 Require longer time to achieve same results as for closed system
APPLICATION OF MAE
APPLICATION OF MAE
 Solvent - Appropriate solvent is very important for obtaining
optimal extraction yields.
FACTORS AFFECTING MAE
 Extraction time - By increasing extraction time, quantity of
analytes is increased but there is the risk of degradation.
FACTORS AFFECTING MAE
 Microwave power - Power must be chosen to minimise the
time needed for extraction.
 However, increased power may cause solvent loss by
evaporation.
 Maximum power used ranges between 600W and 1000W
for closed systems and around 250W for open systems.
FACTORS AFFECTING MAE
 Matrix characteristics - the plant particle size and the status in
which it is presented for MAE can affect the recoveries of
compounds.
 The particle sizes of the extracted materials are generally in the
range of 100m – 2mm.
 Fine powders enhance extraction as they provide a larger
surface area.
FACTORS AFFECTING MAE
FACTORS AFFECTING MAE
 Temperature - temperature should be sufficient to ensure
good solubility of compounds and a good penetration of
solvent in the plant matrix to enhance extraction yield.
 However, it should not be too high enough to degrade the
target compounds.
CONCLUSION
 Chemical analysis of extracts from plant material plays a central
role in development and modernization of herbal medicine.
 MAE has proven to be effective in all aspects compared to
traditional extraction techniques like Maceration/Percolation.
 More research is needed to improve the design and scale up of the
novel extraction systems for their better industrial applications.
REFERENCES
 S. Hemalatha, 2007, Microwave Assisted Extraction – An
innovative and promising Extraction Tool for Medical,
Pharmacognosy Reviews, Vol 1-Issue 1
 Farid Chemat, Giancarlo Cravotto, 2012, Microwave-
assisted Extraction for Bioactive Compounds: Theory and
Practice, Ebook
 Mauricio A. Rostagno, Juliana M. Prado, 2013, Natural
Product Extraction: Principles and Applications, Ebook
 YouTube videos:
 https://www.youtube.com/watch?v=oFSe4HaPggo
 https://www.youtube.com/watch?v=3Em9qU4_2YE

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Microwave Assited Extraction (MAE) techniques of herbal drugs

  • 1. Microwave-Assisted Extraction Techniques for Herbal Drugs Anurag Kumar 12421EN001 2nd November, 2015
  • 2. Contents  Introduction  Microwave theory  Extraction principle  Instruments  Closed vessel  Open vessel  Application of MAE  Factors affecting MAE  Conclusion
  • 3. INTRODUCTION  Microwave-assisted extraction is an efficient method which involves deriving natural compounds from raw plants.  Microwave extraction allows organic compounds to be extracted more rapidly, with similar or better yield as compared to conventional extraction methods.
  • 4.  MAE of anthraquinone in pure alcohol at 60°C for 30 minutes gives a recovery of 65% which results from 3 days maceration in pure ethanol at room temperature.  The advantages that MAE has over other techniques such as Soxhlet are:  Reduction in extraction time  Improved yield  Better accuracy  Suitable for thermolabile substances INTRODUCTION
  • 6. MICROWAVE THEORY  Microwaves are non-ionizing electromagnetic waves of frequency between 300MHz to 300 GHz and positioned between the X-ray and infrared rays in the electromagnetic spectrum.  Microwaves serves two major purposes:  Communication  Energy vectors
  • 7.  The energy vector application is the direct action of waves on materials that has the ability to convert a part of the absorbed electromagnetic energy to heat energy.  As any other EM wave we have two parts of Microwaves  Electric field  Magnetic field MICROWAVE THEORY
  • 8.  In MAE, heating occurs in a targeted and selective manner with practically no heat being lost to the environment as the heating occurs in a closed system.  This unique heating mechanism significantly reduces the extraction time (usually less than 30min) as compared to Soxhlet. MICROWAVE THEORY
  • 9. EXTRACTION PRINCIPLE  Dried plants contain a minute microscopic trace of moisture which serves as target for microwave heating.  High temperature and pressure is generated inside the oven.  High temperature causes dehydration of cellulose which accounts for its reduction of mechanical strength.
  • 10.  The MAE process is as follows:  Microwave radiation  Moisture get heated up  Moisture evaporates  Generation of tremendous pressure on cell wall  Swelling of plant cell  Rupture of the cell  Leaching out of phyto-constituents  This phenomenon can be intensified if the plant matrix is impregnated with solvents with higher heating efficiency under microwave. EXTRACTION PRINCIPLE
  • 11. INSTRUMENTS  There are two types of commercially available MAE systems:  Closed extraction vessels  Focused microwave ovens  The former performs extraction under controlled pressure and temperature.  In the latter, only a part of the extraction vessel containing the sample is irradiated with microwave.
  • 13. INSTRUMENTS  Both systems are available as multi-mode and single-mode.  A multi-mode system allows evenly radiation of sample by random dispersion of microwaves.  Single-mode (aka focused system) allows focused radiation on a restricted zone by a much stronger electric field.
  • 14. INSTRUMENTS  Both multi-mode and focused system comprises of the following four components:  Microwave generator: magnetron which generates microwave energy  Wave guide: propagates microwave to microwave cavity  The applicator: where the sample is placed  Circulator : allow microwave to move in forward direction
  • 15. CLOSED VESSEL  With closed vessel extraction, pressurised microwave assisted extraction is performed under pressure (with or without regulation).  The pressure allows temperatures above boiling points of the solvents to be reached enhancing speed and efficiency.  To avoid overpressure, power, temperature and pressure can be controlled.  When dealing with thermolabile compounds, high temperature causes degradation of analytes. Therefore, the open system is chosen.
  • 16. Advantages of closed-vessel system  Decreased in extraction time  Loss of volatile substances is avoided  Less solvent is required because no evaporation occurs  No hazardous fumes during acid microwave since it is a closed vessel
  • 17. Disadvantages of closed-vessel system  High pressure used poses safety risks  The usual constituent material of the vessel does not allow high solution temperatures  Addition of reagents is impossible since it is a single step procedure  Vessel must be cooled down before it can be opened to prevent loss of volatile constituents.
  • 18. OPEN VESSEL  Extraction is made at atmospheric pressure.  The maximum possible temperature is determined by the boiling point of the solvent at that pressure.  Loss of vapours is prevented by the presence of a cooling system on the top of the extraction vessel that causes condensation of solvent vapours.  Heating is homogenous and efficient.
  • 19. Advantages of open-vessel system  Increased safety  Addition of reagent is possible  Vessels made of various material can be used  Excess solvent can be removed easily  Ability to process large samples  No requirement for cooling down or depressurisation  Low cost of equipment  Suitable for thermolabile products
  • 20. Disadvantages of open-vessel system  This method is less precise than in close-vessel system  The sample throughput is lower as open system cannot process many samples simultaneously  Require longer time to achieve same results as for closed system
  • 23.  Solvent - Appropriate solvent is very important for obtaining optimal extraction yields. FACTORS AFFECTING MAE
  • 24.  Extraction time - By increasing extraction time, quantity of analytes is increased but there is the risk of degradation. FACTORS AFFECTING MAE
  • 25.  Microwave power - Power must be chosen to minimise the time needed for extraction.  However, increased power may cause solvent loss by evaporation.  Maximum power used ranges between 600W and 1000W for closed systems and around 250W for open systems. FACTORS AFFECTING MAE
  • 26.  Matrix characteristics - the plant particle size and the status in which it is presented for MAE can affect the recoveries of compounds.  The particle sizes of the extracted materials are generally in the range of 100m – 2mm.  Fine powders enhance extraction as they provide a larger surface area. FACTORS AFFECTING MAE
  • 27. FACTORS AFFECTING MAE  Temperature - temperature should be sufficient to ensure good solubility of compounds and a good penetration of solvent in the plant matrix to enhance extraction yield.  However, it should not be too high enough to degrade the target compounds.
  • 28. CONCLUSION  Chemical analysis of extracts from plant material plays a central role in development and modernization of herbal medicine.  MAE has proven to be effective in all aspects compared to traditional extraction techniques like Maceration/Percolation.  More research is needed to improve the design and scale up of the novel extraction systems for their better industrial applications.
  • 29. REFERENCES  S. Hemalatha, 2007, Microwave Assisted Extraction – An innovative and promising Extraction Tool for Medical, Pharmacognosy Reviews, Vol 1-Issue 1  Farid Chemat, Giancarlo Cravotto, 2012, Microwave- assisted Extraction for Bioactive Compounds: Theory and Practice, Ebook  Mauricio A. Rostagno, Juliana M. Prado, 2013, Natural Product Extraction: Principles and Applications, Ebook  YouTube videos:  https://www.youtube.com/watch?v=oFSe4HaPggo  https://www.youtube.com/watch?v=3Em9qU4_2YE