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Microwave Assisted Extraction
(MAE)
Presented by
Arun Kumar Gupta
Shubham Rohilla
Seminar on
(FT 702: Techniques in Food Analysis)
Microwaves
• Electromagnetic fields
• 300 MHz to 300 GHz or between wavelengths of 1 cm and 1m.
• Used as information carriers or as energy vectors.
• 2450 MHz and 915 MHz which corresponds to energy output of 600- 700
Watts and 100 Watts (Kingston and Jassie,1998).
MAE is an innovative solvent-extraction technology which involves heating solid
sample-solvent mixtures with microwave energy and the subsequent partitioning
of the compounds of interest from the sample to the solvent.
Principle of microwave
At 2450 & 915 MHz, the electric field swings the orientation of water molecules 2.45 x 10^9 times every
second. Thus, creating an intense heat that quickly as several degrees per second (estimated as 100
Celsius/Second at 4.9 GHz) (Lew et al., 2002).
Dielectric properties of Food
Dielectric constant- It describes the polarizability of the molecule in an electric
field.
Loss factor- It measures the efficiency with which the absorbed microwave
energy can be converted into heat.
Dissipation factor= Dielectric contant
Loss Factor
Magnetron: It is a kind of electron tube within a magnetic field which
propagates high frequency radiant energy. It is consider heart of
microwave. It generates microwave.
Parts of microwave
Principle of MAE
Ionic movement Dipole moment
Working of MAE
1. Open vessel (Monomode)
2. Closed vessel (Multimode)
Open vessel system
This approach is common when the
solvent is nonpolar or microwave-
transparent and the sample is a
biological or agriculture tissue that has
a polar constituent, usually water.
Closed vessel
Used when solvent is polar or microwave absorbent and sample doesn't
posses water.
• The microwave power and temperature used, as both are closely related to
each other. The increase in temperature results in an improved extraction
efficiency as desorption of analyte from active sites in the matrix increases.
• At higher temperatures, surface tension and solvent viscosity decrease and
solvents have higher capacity to solubilize the analytes by improving
sample wetting and matrix penetration respectively.
Parameters which affects MAE process
 Ethanol concentration
 Solvent volume
 Microwave power and
 Extraction time
• Solubility of the analyte in the solvent.
• The mass transfer kinetics of the analyte from the matrix to the solution phase
• The strength of analyte/matrix interactions.
The control factors that direct the extraction of an analyte
The rate of extraction is determined by the diffusion of the analyte to the surface of
the matrix particle. Higher temperatures and swelling of the matrix increase the rate
of diffusion and promote faster extraction kinetics.
Factors to consider when using microwave
assisted extraction method
 Choice of solvent,
 Microwave application time,
 Microwave-power,
 Uniqueness of the matrix
 Effect of contact sample surface area
 Effect of temperature
The choice of solvent
 Solubility of the desired analyte, the solvent-matrix interaction and the property of the
solvent to absorb microwaves (Chen et al., 2008).
 Should have a high selectivity towards the analyte of interest than the other matrix
components and also a good compatibility with further chromatographic analytical steps.
 Solvents which are transparent to microwaves, do not heat up under microwave and those
with good microwave absorbing capacity get heated up faster and enhances the extraction
process.
 Hexane is an example of microwave transparent solvent whereas ethanol is an excellent
microwave absorbing solvent.
 For extraction of volatile oils from several aromatic herbs Solvent free MAE (SFMAE)
has been designed, where the moisture content within the plant matrix itself serves
extraction and no solvent is used.
The matrix
 The ratio of matrix to solvent also plays an important role in extraction (Luque-
Garcia and Luque de Castro, 2003). The solvent volume should be sufficient
enough to immerse the plant matrix completely in the solvent throughout the
entire irradiation process.
 In conventional extraction methods, a higher ratio of solvent volume to solid
matrix gives better extraction yields, whereas in case of MAE a higher solvent:
ratio of solvent to matrix ratio may not give better yield due to non-uniform
distribution and exposure to microwaves.
Microwave Application Time
 The quantity of analyte extracted can be increased with an increase in the
extraction time, but there is an associated risk of degradation of thermo-
labile components (Al-Harahsheh and Kingman, 2004).
 Varying time periods are required for extraction of different matrices, but
exposure of even few seconds have demonstrated to give excellent yields.
Microwave-power
 Low or moderate power with longer exposure is generally selected.
 Although with to the use of high power there is an associated risk of thermal
degradation/deterioration of samples.
• Particle size and the nature of the material will affect the recoveries of the compounds to a
considerable extent. The finer the particles size of the sample the larger the surface area the
better the penetration of microwaves (Huie, 2002).
• Finer particle size of matrix, may sometimes pose a problem during separation of matrix from
solvent after the extraction process. Additional step of centrifugation or filtration can serve as a
remedy to this issue.
Uniqueness of the matrix

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Microwave assisted extraction

  • 1. Microwave Assisted Extraction (MAE) Presented by Arun Kumar Gupta Shubham Rohilla Seminar on (FT 702: Techniques in Food Analysis)
  • 2. Microwaves • Electromagnetic fields • 300 MHz to 300 GHz or between wavelengths of 1 cm and 1m. • Used as information carriers or as energy vectors. • 2450 MHz and 915 MHz which corresponds to energy output of 600- 700 Watts and 100 Watts (Kingston and Jassie,1998). MAE is an innovative solvent-extraction technology which involves heating solid sample-solvent mixtures with microwave energy and the subsequent partitioning of the compounds of interest from the sample to the solvent.
  • 3. Principle of microwave At 2450 & 915 MHz, the electric field swings the orientation of water molecules 2.45 x 10^9 times every second. Thus, creating an intense heat that quickly as several degrees per second (estimated as 100 Celsius/Second at 4.9 GHz) (Lew et al., 2002).
  • 4. Dielectric properties of Food Dielectric constant- It describes the polarizability of the molecule in an electric field. Loss factor- It measures the efficiency with which the absorbed microwave energy can be converted into heat. Dissipation factor= Dielectric contant Loss Factor
  • 5. Magnetron: It is a kind of electron tube within a magnetic field which propagates high frequency radiant energy. It is consider heart of microwave. It generates microwave. Parts of microwave
  • 6. Principle of MAE Ionic movement Dipole moment
  • 7.
  • 8. Working of MAE 1. Open vessel (Monomode) 2. Closed vessel (Multimode)
  • 9. Open vessel system This approach is common when the solvent is nonpolar or microwave- transparent and the sample is a biological or agriculture tissue that has a polar constituent, usually water.
  • 10. Closed vessel Used when solvent is polar or microwave absorbent and sample doesn't posses water. • The microwave power and temperature used, as both are closely related to each other. The increase in temperature results in an improved extraction efficiency as desorption of analyte from active sites in the matrix increases. • At higher temperatures, surface tension and solvent viscosity decrease and solvents have higher capacity to solubilize the analytes by improving sample wetting and matrix penetration respectively.
  • 11. Parameters which affects MAE process  Ethanol concentration  Solvent volume  Microwave power and  Extraction time • Solubility of the analyte in the solvent. • The mass transfer kinetics of the analyte from the matrix to the solution phase • The strength of analyte/matrix interactions. The control factors that direct the extraction of an analyte The rate of extraction is determined by the diffusion of the analyte to the surface of the matrix particle. Higher temperatures and swelling of the matrix increase the rate of diffusion and promote faster extraction kinetics.
  • 12. Factors to consider when using microwave assisted extraction method  Choice of solvent,  Microwave application time,  Microwave-power,  Uniqueness of the matrix  Effect of contact sample surface area  Effect of temperature
  • 13. The choice of solvent  Solubility of the desired analyte, the solvent-matrix interaction and the property of the solvent to absorb microwaves (Chen et al., 2008).  Should have a high selectivity towards the analyte of interest than the other matrix components and also a good compatibility with further chromatographic analytical steps.  Solvents which are transparent to microwaves, do not heat up under microwave and those with good microwave absorbing capacity get heated up faster and enhances the extraction process.  Hexane is an example of microwave transparent solvent whereas ethanol is an excellent microwave absorbing solvent.  For extraction of volatile oils from several aromatic herbs Solvent free MAE (SFMAE) has been designed, where the moisture content within the plant matrix itself serves extraction and no solvent is used.
  • 14. The matrix  The ratio of matrix to solvent also plays an important role in extraction (Luque- Garcia and Luque de Castro, 2003). The solvent volume should be sufficient enough to immerse the plant matrix completely in the solvent throughout the entire irradiation process.  In conventional extraction methods, a higher ratio of solvent volume to solid matrix gives better extraction yields, whereas in case of MAE a higher solvent: ratio of solvent to matrix ratio may not give better yield due to non-uniform distribution and exposure to microwaves.
  • 15. Microwave Application Time  The quantity of analyte extracted can be increased with an increase in the extraction time, but there is an associated risk of degradation of thermo- labile components (Al-Harahsheh and Kingman, 2004).  Varying time periods are required for extraction of different matrices, but exposure of even few seconds have demonstrated to give excellent yields. Microwave-power  Low or moderate power with longer exposure is generally selected.  Although with to the use of high power there is an associated risk of thermal degradation/deterioration of samples.
  • 16. • Particle size and the nature of the material will affect the recoveries of the compounds to a considerable extent. The finer the particles size of the sample the larger the surface area the better the penetration of microwaves (Huie, 2002). • Finer particle size of matrix, may sometimes pose a problem during separation of matrix from solvent after the extraction process. Additional step of centrifugation or filtration can serve as a remedy to this issue. Uniqueness of the matrix