Professional Documents
Culture Documents
Advisory Committee
Chair
(Associate Professor Jaturapatr Varith , Ph.D.)
..................../.................../................
Committee
(Associate Professor Somkiat Jaturonglumlert , Ph.D.)
..................../.................../................
Committee
(Assistant Professor Kanjana Narkprasom , Ph.D.)
..................../.................../................
Committee
(Assistant Professor Nukrob Narkprasom , Ph.D.)
..................../.................../................
Page
TABLE OF CONTENTS ..................................................................................................................... D
List of Tables.....................................................................................................................................G
List of Figures ................................................................................................................................... H
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CHAPTER 1 ......................................................................................................................................... 1
INTRODUCTION ................................................................................................................................. 1
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Page
Table 1 Mathematical models for thin-layer drying of C. papaya leaves........................16
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List of Figures
Page
Figure 1. Conceptual framework of the research. .................................................................12
Figure 2. Setup of the process for MD. .....................................................................................14
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CHAPTER 1
INTRODUCTION
C. papaya is a plant that grows in the tropical and subtropical regions of the
world, the different parts of which possess numerous nutrients (Santana et al., 2019).
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Its leaf is among its widely sought parts due to its antidiabetic and cholesterol-
reducing (Juarez-Rojop et al., 2012), anti-cancer (Hoque et al., 2015), antimicrobial
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(Baskaran et al., 2012), and anti-dengue (Sharma et al., 2019) properties, among many
others. These properties are mostly attributed to the presence of food fibers and
polyphenolics, such as flavonoids and saponins, in large amounts (Santana et al.,
2019). Despite its medicinal and therapeutic advantages, however, it is of little to no
appeal due to its bitter taste owing to its saponin content (Syed Amran et al., 2018).
Thus, it rarely finds suitability for use in culinary, the reason for it being rather utilized
in extract form.
In past studies employing extraction of C. papaya leaf extract, decoction was
the most widely used. This is typically because of its actual use in household settings
as a traditional method of preparing natural treatment and cure for diseases. On the
one hand, this extraction method is beneficial in that boiling can increase the level
of phytochemicals present in the plant (Gunathilake et al., 2018). On the other
hand, however, it is detrimental to the environment because of the high input of
both water and energy needed for optimal extraction when adopted to industrial
settings. It is for this downside that researchers have been exploring non-
conventional extraction methods in recent years. Further cemented by the advent
of the Sustainable Development Goals (SDGs), there seems to be a race for the
discovery of novel extraction methods that increase the industrial value of plants,
while at the same time, pose a reduced need for water and energy inputs. Among
the recent technologies studied as of late in terms of their applicability for
sustainability as extraction methods are microwave, ultrasound, pulse electric field,
instant controlled pressure drop, and supercritical fluid. Although these technologies
2
have been heavily researched on for more than three decades, it was only until
recently that they are explored on the basis of sustainable process design (Chemat
et al., 2017).
Aside from extraction, drying also helps increase the industrial value of plants
due to increase in phytochemical content catalyzed by elevated temperatures. For
instance, in a study on chrysanthemum flower heads (from two developmental
stages) (Yuan et al., 2015), it was found that oven-drying at 60ºC and 70ºC yielded
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the best quality parameters, including high phytochemical contents, from within a
temperature range of 40ºC to 120ºC. However, this may not always be the case for
all plants. Some plants find a reduction in phytochemical contents beyond 70ºC,
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while others find an increase in phytochemical contents even beyond the same
temperature. Thus, it is important to note that the impacts of heating on the changes
in phytochemical contents are dependent on the plant species and drying method
(Gunathilake et al., 2018).
Among the drying methods, microwave drying (MD) is considered to be one of
the most advantageous so far due to its efficiency. In just a matter of minutes, a
high amount of moisture can be removed from the material because the microwaves
selectively target it, not only heating the outer surface but also the inner parts (M.
Youssef and Mokhtar, 2014). On the downside, this drying method still lacks more
solid information as to its scalability for industry adoption. Meanwhile, using certain
assumptions and specific data collected from industrial companies through surveys,
industrial microwave-assisted extraction (MAE) was found in a study by Plazzotta et
al. (Plazzotta et al., 2020) to be less impactful than ultrasound-assisted extraction
(UAE) in terms of both greenhouse gas emissions and energy requirements despite its
higher energy density requirements in laboratory scale. This suggests a good future
for MAE which might also be the case for MD since they both employ the same
principles of microwave application.
For decades now, both MD and MAE have been frequently exploited in
studies on retention and extraction of phytochemicals from leaves. Among the most
notable recent studies were on coriander leaves (Hihat et al., 2017), lemon myrtle
leaves (Saifullah et al., 2019), purslane leaves (M. Youssef and Mokhtar, 2014),
3
Vernonia amygdalina L. leaves (Alara et al., 2018), Perilla frutescens leaves (Shao et
al., 2012), young barley leaves (Gao et al., 2016), and parsley leaves (El-Hadidy and
Mostafa, 2019), among many others. This exploitation is in large part driven by the
aim of achieving the SDGs by 2030.
The 2030 Agenda for Sustainable Development launched by the United
Nations in 2015 consists of goals for each Member State to achieve within the 15-
year timeframe. These goals are interconnected and consider the environmental,
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economic and social aspects of the planet in order to meet the needs of every
human being at present without jeopardizing the welfare of future generations
(Schaefer and Crane, 2005). Nine of the 17 SDGs are directly related to the global
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food and beverage system. These are: SDG 2 Zero Hunger; SDG 3 Good Health and
Well-being; SDG 6 Clean Water and Sanitation; SDG 7 Affordable and Clean Energy;
SDG 9 Industry, Innovation and Infrastructure; SDG 12 Responsible Consumption and
Production; SDG 13 Climate Action; SDG 14 Life Below Water; and SDG 15 Life On
Land. The entire food supply chain, from primary to tertiary processing (including
distribution), contributes a total of approximately 13.7 billion metric tons of carbon
dioxide equivalents (CO2eq) to date (Poore and Nemecek, 2018). Considering the
processing side alone, the conversion of raw materials to finished food and beverage
products is already an energy-intensive process. As a result, researchers from both
academe and industry alike have been searching for ways to reduce water and
energy inputs, and hence, greenhouse gas emissions.
Although much work has already been done on MD and MAE, only a few has
considered the sustainability potential of these technologies. At the same time, little
to no information is available on the application of both MD and MAE on C. papaya
leaves.
The general aim of this research is to obtain C. papaya leaf extract through
microwave-based processing methods for use as a functional food ingredient.
Specifically, it aims:
4
1.4 Keywords
CHAPTER 2
LITERATURE REVIEW
other tropical regions of the world due to its appealing fruit, but its other plant parts
are also now being used for various purposes (Sharma et al., 2019). It is highly
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inflammatory, and cardio-protective properties (Akhtar et al., 2019; Patel et al., 2012).
Lastly, flavonoids were found to have blood cholesterol-reducing properties, as well
as, antioxidative, anti-hypertensive, anti-microbleeding, antibacterial, and anti-dengue
properties, among many others (Akhtar et al., 2019; Ghasemzadeh and Ghasemzadeh,
2011; Kumar and Pandey, 2013). Lastly, saponin also has medicinal and therapeutic
benefits, including antidiabetic properties (El Barky et al., 2017). These properties are
only just a portion of the many in different phytochemicals, and it is for this reason
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that phytochemicals are being considered and explored for use in functional foods.
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and non-polar compounds alike, as well as, allows repetitive use of organic solvents
(Routray and Orsat, 2012). Due to its environment-friendly advantages, it has been
described (Llompart et al., 2019) as “an automated green extraction technique”.
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These advantages are in large part due to the microwave radiation that is capable of
selective heating.
MAE works by heating the water molecules (and other polar molecules)
inside the material, causing them to vaporize. When this happens, plant cell walls
break and release phytochemicals into the solvent (Destandau et al., 2013). The
effectivity of MAE depends on several factors such as irradiation time, temperature,
material-to-solvent ratio, solvent concentration, and microwave power level (Alara et
al., 2018), as well as, other solvent properties and system attributes (Bagade and
Patil, 2021). Because the effectivity of MAE is determined by various parameters at
play, several optimization methods have been employed to maximize extraction
yield. Among the experimental designs employed in past studies are orthogonal test
(Niu et al., 2020), box-behnken design (Deng et al., 2019; Filip et al., 2017), and face-
centered central composite design (Weremfo et al., 2020).
In a study by Lovric et al. (Lovrić et al., 2017), they found that both total
phenolic content and antioxidant capacity were improved by a higher extraction
temperature. As for extended extraction time, however, only total phenolic content
was improved, and not antioxidant capacity. The same was the case for another
study (Sharma et al., 2020) in that the total phenols reached its maximum
extractable amount and the antioxidant activity slightly increased when the
irradiation time was increased from 30 sec to 90 sec. Moreover, in terms of energy
consumption, laboratory-scale setup seems to show promise. However, a number of
8
reviews have found that this setup has not always considered the scale up aspects
(Rosa et al., 2018). Nonetheless, a study on peony seed oil extraction (Sun et al.,
2016) considered energy consumption from a different angle. Manipulating the
amount and composition of solvents as extraction agents, they found that using
ethanol and hexane mixture is a successful energy consumption reduction method.
The downside of this, however, is that hexane is an environmentally toxic substance.
Although MAE has many advantages to offer, it also has disadvantages. For
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the most part, the heating it produces is not uniform, sometimes resulting in
overheating of extract. Another disadvantage is the need for filtration (Al Jitan et al.,
2018). In closed-vessel systems, an additional disadvantage is the risk involved when
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operating at high pressures, as well as, the limited capacity (Tatke and Jaiswal, 2011).
The development of MAE dates back to as early as the 1980’s when it was
first used by Ganzler et al. To date, it has encountered several modifications, such as
dynamic microwave-assisted extraction (DMAE), focused microwave Soxhlet
extraction (FMSE), and solvent-free microwave extraction (SFME) (Routray and Orsat,
2012).
Water has the highest dielectric constant at 20ºC (=78.5) when compared with
hexane (=1.89), toluene (=2.4), dichloromethane (=8.9), acetone (=20.7), ethanol
(=24.3), and methanol (=32.6), thus making it a good extracting solvent (Nn,
2015),(Kaufmann and Christen, 2002). It is cheap, nontoxic, environment-friendly and
highly polar. On the contrary, it may cause hydrolysis and its heating an energy-
intensive process (Abubakar and Haque, 2020). Another downside of it is that not all
extracts are soluble in it therefore only a selected number of natural substances can
be isolated and in limited amounts. For instance, in a study on extraction of
bioactive compounds from S. buxifolia branches (Truong et al., 2019), they found
that the best solvent to use was methanol because despite the lower dielectric
constant than that of water, it has both polar and non-polar groups which are
capable of bonding both hydrophilic and hydrophobic compounds. Fortunately,
9
flavonoids and saponins are both soluble in water (Ferreira and Pinho, 2012; Savage,
2003), but only some parts and/or types are hydrophilic.
depended on the drying method and condition. Weiguang and Hazel, 2011 study on
selected herbs also agreed when they found that drying can improve the total
polyphenol (TPP) and Trolox equivalent antioxidant capacity (TEAC), thus increasing
its bioavailability and absorption. An additional advantage of drying is that it also
eliminates the interference caused by water with the solvent (Altemimi et al., 2017).
On the other hand, a significant decrease in phenolic compounds in air-dried and
oven-dried A. zerumbet leaves at 70ºC was observed in Elzaawely and Tawata’s
study (Elzaawely and Tawata, 2011). This finding was in agreement with Nadi, 2017,
Nguyen and Le, 2018 and Saifullah et al., 2019 studies that drying has the possibility
to harmfully affect some natural components that are sensitive to heat.
Among the drying methods, microwave drying (MD) is the best due to rapid
volumetric heating via dipole rotation and ionic conduction (Sujinda et al., 2020). In
a study on microwave-dried coriander leaves (Hihat et al., 2017), it was found that
MD at 900 W was faster than oven-drying (OD) at 120ºC. In addition to the drying
rate, total phenolic content (TPC), total flavonoid content (TFC), and radical
scavenging activity also showed a positive change after MD. On the contrary, a study
on drying lemon myrtle leaves at different conditions showed freeze-drying (FD) to
be the best method in increasing TPC, TFC, proanthocyanidins, gallic acid, and
10
hesperetin (Saifullah et al., 2019). Despite these findings, however, MD was still
suggested for industrial scale drying due to time and energy efficiency.
In a study on purple basil leaves (Altay et al., 2019), they found that shade-
drying (SD), FD and conventional drying (CD) were significantly longer than MD.
Finding the best-fit mathematical models for SD and MD, Modified Henderson and
Pabis, and Page, respectively, were selected. In terms of effective moisture diffusivity
(Deff), increasing the microwave power level exhibited increased Deff. In terms of
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economics, MD exhibited the highest specific moisture extraction rate (SMER) and
moisture extraction rate (MER), as well as, lowest specific energy consumption (SEC).
These findings were in agreement with Varith et al., 2007 study on combined
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A review by Patel et al. (Patel et al., 2014) defines green process engineering
as “the design, commercialization, and use of processes and products, which are
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feasible and economical while minimizing generation of pollution at the source and
risk to human health and the environment.” Emphasizing further, they noted that
the development phase is crucial in impacting human and planet health while also
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CHAPTER 3
RESEARCH METHODOLOGY
This research will be divided into two parts – Part 1: microwave drying (MD),
and Part 2: microwave-assisted extraction (MAE) – as shown in Figure 1. The
investigation of the sustainability potential of the MD-MAE process will be done
towards the end and will integrate the two parts.
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– with the initial weight to be determined during the set up. Drying will be
carried out in two modes: (1) with constant weight as the endpoint, and (2)
with color change as the endpoint. A fresh batch of sample will be used for
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each time duration with the weight monitored at 30-sec intervals from the
beginning using a 1-mg precision analytical balance (Citizon CX 265,
Philippines), as depicted in Figure 2. Prior to weighing, the dried sample will
be equilibrated using a desiccator. Weighing will be completed within 10 sec
as in the method of Alibas (Alibas, 2014) and Potisate and Phoungchandang
(Potisate, 2015), by weighing the plastic container containing the sample. This
plastic container will be perforated and elevated from the glass turntable to
enable moisture to escape easily from the product. To assist the removal of
moisture, a suction fan will be attached to the outermost wall of the
microwave oven where existing orifices are already located. For mode 1,
drying will be continued until a constant weight is reached for three
consecutive measurements. For mode 2, drying will be continued until a
color change is observed. This will be done to see which mode will yield
higher flavonoids and saponins. The temperature of the sample will also be
measured quickly using an infrared thermometer at the center point before
the sample will be removed from the microwave oven for weight
measurements to also provide data on the temperature profile of the drying
process. From this experiment, the moisture content (via weight reduction)
will be obtained.
14
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Once the optimal drying mode and range that yield good flavonoids
and saponins content is determined, the laboratory experiments will be run
at Maejo University.
Mt −Me
MR =
Mi −Me
(1)
Where MR is the Moisture Ratio; Mi and Mt are the initial moisture content
and moisture content at time t, respectively; and Me is the equilibrium
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moisture content.
The mathematical models that will be fitted with the experimental
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∑N
i=1(MRpre,i −MRexp,i )
2
R2 = 1 − ∑N 2 (2)
i=1(MRpre −MRexp,i )
1 1⁄2
RMSE = [ ∑N
I=1(MR exp,i − MR pre,i )2]
N
(3)
16
Modified Page
2 MR = exp[−(kt)n ] (5)
(Overhults et al., 1973)
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Logarithmic
3 MR = a exp(−kt) + c (6)
(Yagcioglu et al., 1999)
Two-term
4 MR = a exp(−k 0 t) + b exp (−k1 t) (7)
(Henderson, 1974)
Two-term exponential
5 (App. of diff.) MR = a exp(−kt) + (1 − a) exp (−kat) (8)
(Sharaf-Elden et al., 1980)
Midilli et al.
6 MR = a exp(−kt n ) + bt (9)
(Midilli et al., 2002)
8 Deff ×π2
ln(MR) = ln ( 2 ) − (
π 4L2s
)t (10)
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−Ea ×m
Deff = D0 exp (
P
) (11)
content, the initial moisture content of the fresh C. papaya leaves will also
be measured prior to beginning the drying experiments.
W per 10 g of leaf powder (because beyond this, the flavonoids content will
begin to decrease). The extracts will be filtered and concentrated using
rotary vacuum evaporator at 50 rpm and 50ºC for 15 min, exactly as in the
method by Waziiroh et al., 2018.
3.1.8 Total flavonoids content (TFC) and Total saponins content (TSC)
The C. papaya leaf ethanolic extract will be sent to an analytical
laboratory for determination of TFC and TSC through UV-Vis spectroscopy for
preliminary studies and through FTIR spectroscopy for final study. The
procedure for this will depend on the laboratory’s official procedure for
phytochemical analysis.
P×t
SEC =
m
(12)
Where SEC is the energy consumption per mass of sample (kWh/g), P is the
average actual power input (kW), t is time elapsed (h) and m is the sample
mass (g).
19
The actual power input will be measured using a power meter (OMNI
MMA-D02P, Philippines) at 30-s intervals throughout the process to obtain the
average.
3.1.10 Confirmation of the optimum condition for high TFC and TSC
After determining through FTIR spectroscopy the microwave drying
treatment that yields the highest TFC and TSC, a confirmation experiment will
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be performed for that specific treatment. The microwave power level and
drying time from the final study will be repeated to confirm the results. In
this confirmation test, the residual moisture content, TFC and TSC will again
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as solvent. With the flavonoids and saponins yield obtained from this, the
aqueous MAE extraction parameters will be manipulated to reach, if not
exceed, the same yields. The amount of obtained crude extract will be
recorded. As in 3.1.7, the extracts will be filtered and concentrated using
rotary vacuum evaporator at 50 rpm and 50ºC for 15 min.
V × CF
SEC =
m
(13)
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Where SEC is the energy consumption per mass of sample (kWh/g), V is the
amount of LPG consumed (L), CF is the conversion factor (kWh/L) and m is
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Lastly, the efficiency of the overall process from drying to extraction will be
critically analyzed in terms of amount of valorized extract obtained from an amount
of fresh C. papaya leaves, using Equation 14.
22
For economic aspect, the total amount and cost of resources used (water,
energy etc.), SEC in kWh/g of extract (as in Equations 12 and 13), and estimated
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Where GHG Emissions in CO2 equivalents is in metric tons CO2, ECe is the total
electrical energy consumption (kWh), and 7.09x10-4 is the emission factor (metric tons
CO2/kWh) according to the EPA (EPA, 2020).
Where GHG Emissions in CO2 equivalents is in metric tons CO2, ECt is the total
thermal energy consumption (kWh), 0.03 is the conversion factor (therm/kWh), and
0.0053 is the emission factor (metric tons CO2/therm) according to the EPA (EPA,
2020).
For Part 1, MD will be compared with HAD, and for Part 2, MAE with HWE.
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MJU iThesis 6303307001 proposal / recv: 21052564 17:09:44 / seq: 2
CURRICULUM VITAE
WORK EXPERIENCE Love has a total of about three and half years of
professional work experience. The first five months was as
MJU iThesis 6303307001 proposal / recv: 21052564 17:09:44 / seq: 2