Food Engineering – III

ENG- 311
Diksha Singh

120057 (A2)

B.Tech’24

Practical No. 3

1. Title: Microwave Assisted Extraction (MAE) Process

2. Objective:

a. Study the Microwave Assisted extraction apparatus

b. Study the Microwave Assisted technique.

3. Theory:

Principle
MAE is based on the interaction of a dielectric polar substance (such as water) with a fast-
oscillating electric field generated by microwaves, which generates heat due to friction
caused by inter- and intramolecular movement. The heat causes the cell to produce water
vapour, which leads to cell rupture and further leakage and release of intracellular
components via an electroporation effect.

The main parameters to consider for MAE are extraction time, temperature, dielectric
properties of the process mixture, solid/liquid ratio, and solvent type and concentration.

Dielectric constants of common solvents

solvents Dielectric constants

hexane 1.89
heptane 1.92
dichloromethane 8.9
2-propanol 19.9
acetone 20.7
 ethanol 24.3
methanol 32.6
acetonitrile 37.5
water 78.3

Advantages

 Surprisingly, less extraction time was required. The extraction time ranges from a few
seconds to a few minutes (15-20 min).
 The amount of solvent used is reduced. MAE requires only a few millilitres of
solvent.
 The extraction yield has increased.
 Better precision and accuracy as a result of the instrument's automation.
 This is advantageous for thermos labile constituents.
 Heavy metals and pesticide residue in minute traces can be extracted from a few
milligrams of plant sample.
 It provides agitation during extraction, which improves the mass transfer
phenomenon.

Disadvantages

 Selectivity, only polar molecules can be heated.

 One significant disadvantage of this method is the high maintenance cost in
commercial settings.
 Lipid oxidation may occur as a result of energy.

Procedure:

 Microwaves are non-ionizing electromagnetic radiation with frequencies ranging from

0.3 to 300 GHz and typically extracted at 2.5 to 75 GHz in natural products. The
efficiency of microwave energy is largely determined by the solvent content, plant
material, and microwave power applied.
 The microwave energy heating principle is based on the direct effects of microwaves
on material molecules. In both the solvent and the sample, two mechanisms convert
electro-magnetic energy to calorific energy: ionic conduction and dipole rotation. In
 many applications, these two mechanisms operate concurrently, effectively converting
microwave energy to thermal energy.
 Microwave heating, unlike traditional conductive heating, is volumetric; the entire
sample is heated at the same time. The temperature gradient is reversed in comparison
to conventional heating because heating occurs in the centre of the solvent-matrix
mixture, whereas conventional heating heats the surface first. There is no inertia, and
the temperature in the medium quickly becomes homogeneous.
 When an electromagnetic field is applied, ions migrate electrophoretically, resulting
in ionic conduction. Because the direction of the ions changes as many times as the
field changes sign, the resistance of the solution to this flow of ions and collisions
between molecules will result in friction and thus heat the solution. Furthermore,
dissolved ion migration increases solvent penetration into the matrix, facilitating
target compound solvation.
 Dipole rotation refers to the alternative movement of polar molecules with dipole
moments (either permanent or induced by the electric field) that attempt to align with
the electric field. As the field weakens, thermal disorder returns, resulting in the
release of thermal energy. At 2450 MHz (the frequency used in commercial systems),
the molecules align and then return to disorder 4.9 x 109 times per second, resulting
in rapid heating.
 The stronger the oscillation in the microwave field, the greater the molecule's dipole
moment. This dipole rotation causes the weak hydrogen bounds to be broken. The
viscosity of the medium reduces this mechanism by influencing molecular rotation.
 Heat generation in the sample by the microwave field requires the presence of a
dielectric compound, and heat release is observed only if the sample has dielectric or
conducting losses when exposed to microwave irradiation. This ability of a solvent to
absorb microwave energy and convert it into heat is partly dependent on the
dissipation factor, 𝑇𝑎𝑛 𝛿

′′
𝜀
𝑇𝑎𝑛 𝛿=
𝜀

Where,

𝜀′ is dielectric constant

And 𝜀′ ′ is dielectric loss factor.

The greater the dissipation factor, greater the thermal energy.

Polar solvents, such as water, have high dielectric losses; microwaves that have been strongly
absorbed will affect their permanent dipole moment. Non-polar solvents, such as hexane, do
not heat up when exposed to microwaves and are therefore referred to as microwave-
transparent solvents.

Principle components of a microwave device:

The microwave extraction assembly is made up of four major parts.

A microwave generator, also known as a magnetron, is in charge of producing microwaves.

A wave guide is used to direct microwave propagation from the source to the microwave
cavity.

The third component is the applicator, which holds the sample holder and the sample.

The Circulator, which only regulates microwave movement in the forward direction, is the
next component.

In multi-mode systems, the applicator is a closed cavity within which a random dispersion of
microwaves occurs. Beam reflectors or turntables aid in the uniform distribution of
microwave energy inside the cavity, regardless of sample placement position.

The microwave waveguide serves as the applicator in focused microwave systems, and the
extraction vessel is placed directly in the cavity. Only a few inches of the vessel's bottom are
exposed to microwaves, and because glass is microwave-transparent, the upper region of the
vessel remains cool. As a result of the microwave's inbuilt design, an effective condensing
mechanism result.

Diagram:
Conclusion:

Microwave assisted extraction is a focused and targeted method of plant metabolite extraction
that can be easily combined with other analytical methods. The instrument's automation
makes it even easier to handle. MAE has grown rapidly over the last decade, and it has
proven to be effective in all aspects when compared to traditional extraction procedures. It is
further reasoned that a country like Pakistan, which is facing energy crisis problems for its
economy, requires such extraction systems for all industries that involve modern applications
to reduce overall energy consumption. More research is expected to be conducted in order to
remove technical barriers and improve the outline and scale-up of the novel extraction
frameworks.
Case Study.

1. Title of research paper:

Volatiles of Fresh and Commercial Sweet Red Pepper Pastes: Processing Methods and
Microwave Assisted Extraction

2. Authors, name of the journal, publication year:

Fahrettin Gogus, Mustafa Z. Ozel, Hasene Keskin, Derya Kocak Yanık & Alastair C. Lewis
International Journal of Food Properties

Published online:08 Apr 2015

3. Brief discussion of work:

Abstract—

Flavor compounds were extracted from fresh red pepper fruit, as well as traditional and
industrially made pepper pastes, using microwave-assisted hexane or water extraction. There
were 79 compounds identified in total, including 15 alcohols, 14 terpenes, 13 aldehydes, 12
ketones, 7 fatty acids, 6 fatty acid esters, and 6 browning reaction products. Microwave-
assisted hexane extraction from the traditionally made pepper paste gave the highest number
of volatiles.

Keywords: Microwave, Extraction, Pepper paste, Volatiles, Gas chromatography.

INTRODUCTION

Pepper paste is used as a colouring and flavouring ingredient in a variety of dishes. Aside
from its use as an ingredient, studies have shown that fermented pepper paste has health
benefits such as anti-diabetic effects.

Microwave-assisted extraction (MAE) has received a lot of attention as a potential alternative

to traditional extraction methods, owing to significant time, solvent, and energy savings.
Using MAE systems, researchers investigated the extraction of volatiles from various
products. However, no research has been conducted to identify the volatile compounds found
in both industrially and traditionally produced pepper paste.
EXPERIMENTAL WORK

Ripe, fresh, and undamaged red pepper (Capsicum annum L.) fruits and industrially produced
pepper paste were purchased from a Turkish market.

Preparation of the sample

Fresh red pepper seeds and stems were separated, and peppers were cut into small (5 mm)
pieces. The moisture content of all fresh and paste samples was determined using a vacuum
oven at 70°C, and weight loss was reported as moisture.

The pepper samples had a final moisture content of less than 10%.

MAE

The extractions were carried out in an open-vessel system linked to a condenser. At

atmospheric pressure, a microwave operating at 2450 MHz with dynamic power control was
used. A constant temperature was used.

MAEs of volatiles from fresh red pepper pastes were performed under optimised reaction
conditions with the dynamic power mode set to fixed power (250 W) for 10 minutes.

The samples (20 g) were heated in an open system microwave at 250 W by adding solvent
(40 mL) into 150 mL vessels. As extraction solvents, water and n-hexane were used. Water
extraction temperatures were 95°C and n-hexane extraction temperatures were 55°C.

In the case of n-hexane extraction, the filtrates were dried over anhydrous MgSO4, and the n-
hexane was evaporated using a rotary vacuum evaporator until only 2 mL of hexane
remained.

RESULTS AND DISCUSSION

The microwave technique was used to extract the volatile components of fresh sweet red
pepper and pastes. Modern MAE techniques have higher extraction efficiency because they
operate at much higher temperatures and pressures and require less extraction time.

A range of fatty acids and their esters (64.39%), ketones (10.07%), aldehydes (8.11%),
alcohols (5.98%), and terpenes (2.72%) were found to be present in the volatiles of hexane
extracted fresh red peppers. The major components identified in the fresh red pepper were
palmitic acid (15.59%), oleic acid (14.27%), linoleic acid (10.84%), linolenic acid ethyl ester
(9.03%), 9-Octadecenal (4.49%), and β-ionone (4.29%). In this study, the actual number of
components extracted from each type of sample was greater than 80. The volatiles extracted
from fresh red pepper using microwave-assisted water extraction differed greatly in quantity
and concentration from those extracted using hexane. This could be explained by changes in
component solubility in water.

CONCLUSION

When compared to hexane, microwave-assisted water extraction of the samples resulted in a

decrease in the number of volatile compounds and their amounts. The number of volatile
compounds discovered through microwave-assisted water extraction of fresh pepper,
industrially produced pastes, and traditionally produced pastes was 22, 30, and 29,
respectively. These figures were 42, 39, and 64 when hexane was used as the solvent. This
could be explained by the fact that these compounds are less soluble in water.