Professional Documents
Culture Documents
FYP Report Kavya - RP - SAS
FYP Report Kavya - RP - SAS
August 2023
Project number: SAS-2023-2310-0044
Table of Contents
Table of Contents ii
Abstract iii
Acknowledgements iv
List of Figures 2
List of Tables 3
Chapter 1 4
Introduction 4
Chapter 4 Conclusion 21
References………………………………………………………………….22
Project number: SAS-2023-2310-0044
Abstract
Lycopene microcapsules were prepared by a spray drying system method using plant-based proteins
(GA and GB) and pectin. Where lycopene was mixed with soya bean oil to enhance the oxidative
stability/ bioavailability of lycopene. Effects of various factors such as, the ratio of GA to GB, the
amount of lycopene oil, pectin, homogenization time, inlet temperature, pH of the feed and yield of
encapsulation were examined. Four best samples with yield ranging from 35.53% to 49.50% were
taken for further analysis based on their yield and colour. The results showed that encapsulation yield
were affected by the homogenizing time, ratio of GA to GB, amount of lycopene oil added. The
optimal conditions were determined as follows: 300ml GA, 7.5g GB, 3.75g pectin, 6.2 pH and inlet
temperature of 160C. Further, the scanning electron microscope (SEM) analysis showed that the
microencapsulated lycopene had a regular spherical shape with a particle size distribution of 3-8 um.
This study can be used to enhance the application of lycopene in the food industry.
Acknowledgements
First and foremost, I would like to extend my deepest appreciation to the supervisor Dr
Chiradip Chatterjee for his guidance, expertise and continuous encouragement
throughout this study. His feedback and unwavering support helped in completing the
study successfully.
I would also like express my heartfelt gratitude to the TSOs Ms Nuratikah Bazilah and
Ms Amirah Ayub for always being supportive, for guiding the team and teaching the
proper use of equipment. I also want to thank all the other TOs who supported with other
quality control tests.
Last but not least, I want to thank my teammates for being extremely corporative and
supportive to one other. The enthusiasm and collaborative team spirit created a positive
environment. The team’s commitment to the study ensured we completed the study on
time. I am privileged to have had the opportunity to work with such dedicated
individuals.
Project number: SAS-2023-2310-0044
List of Figures
Figure 1. Skeletal structure of lycopene 3
Figure 2. Weighing lycopene mixed with soy bean oil 4
Figure 3a. Weighing GB 5
Figure 3b. Mixing GA, GB and pectin using a spatula 5
Figure 4. Measuring pH of the liquid feed 6
Figure 5. Spray drying in process 7
Figure 6a. Microencapsulated lycopene in the cyclone 8
Figure 6b. Collecting dry microencapsulated powder 8
Figure 6c. Weighing the dry microencapsulated powder8
Figure 7. Measuring the moisture content of the sample8
Figure 8a. Coating the SEM stub with platinum in vacuum 9
Figure 8b. Scanning electron microscope (SEM) 9
Figure 9a. Electron microscope 10
Figure 9b. Microencapsulated powder samples placed on the slides 10
Figure 9c. Zoomed image of the microencapsulated powder under the light microscope 10
Figure 10. Measuring the viscosity of the samples 11
Figure 11. Water activity meter 11
Figure 12. Sample I- showing the two different colors 13
Figure 13. (A) Sample I (B) Sample H2 13
Figure 14. Sample 3 15
Figure 15. Sample H1 16
Figure 16. Sample H2 16
Figure 17. Sample I 17
Figure 18a. Stability test observation before placing the samples in the stability chamber 17
Figure 18b. Stability test observation after taking the samples from the stability chamber 17
List of Tables
5
Project number: SAS-2023-2310-0044
Chapter 1
Introduction
Spray Drying is one of the most common methods used for microencapsulation in
food industry[2]. The process involves converting a liquid feed into dry powder by
atomization. Where the liquid feed is a homogenized mixture of the core material and
the coating material[3]. The liquid emulsion is fed into the feed system and is passed
into the drying chamber where the liquid is atomized into tiny droplets using the spray
nozzle, creating a large surface area for rapid evaporation. Hot air is concurrently
introduced into the chamber facilitating the evaporation of the liquid from the
droplets, leaving behind dry particles in the cyclone and the collecting beaker[3].
The liquid feed is a homogenized mixture of the core material and the coating
material where the core material is lycopene. Lycopene is a red carotenoid, found in
various fruits and vegetables such as, tomato, watermelon and pink grape fruit giving
them their red characteristic[4]. Lycopene has gained significant attention in recent
years to have potent antioxidant properties, which means lycopene helps the body’s
cells from the damage caused by free radicals, free radicals can lead to oxidative
stress which can cause chronic diseases such certain cancers, cardiovascular disorders
[4][5]. By neutralizing free radicals, lycopene helps reduce the risk of cellular damage
and related health issues. However, despite the benefits of lycopene the of the
presence of unsaturated bonds in molecular structure of lycopene makes it highly
unstable prone to attack by oxygen molecules, leading to the formation of free
radicals [6].
The conjugated system (fig. 1) in lycopene also contributes to its vibrant red color.
However, these same double bonds [7] also make it vulnerable to degradation by
light, particularly UV light, which can break down the molecular structure and reduce
its color intensity and efficacy [8]. Moreover, lycopene's chemical structure can
6
Project number: SAS-2023-2310-0044
7
Project number: SAS-2023-2310-0044
(a) (b)
Figure 3. (a) Weighing GB (b) mixing GA, GB and pectin using a spatula
8
Project number: SAS-2023-2310-0044
9
Project number: SAS-2023-2310-0044
the experiment, which could influence the microencapsulation process. The liquid
feed is then loaded into the feeding system of the spray dryer where pump is set at
10% and nozzle cleaner at 6. The liquid feed will go through atomization and form
into micro droplets, a these microdroplet pass the drying chamber the solvent in the
encapsulating mixture evaporates rapidly due to the high temperature in the system.
This process leads to the solidification of the encapsulating agents (GA, GB, and
pectin) around the lycopene droplets, forming microcapsules that encase the active
ingredient. The spray-dried micrcapule are then separated from the drying air in the
cyclone chamber and collection vessel.
10
Project number: SAS-2023-2310-0044
amounts of the samples were placed on one surface of a double- sided adhesive tape
ensuring that the sample sticks to the SEM stub. The SEM stub is coated with
platinum under vacuum using a JOEL JFC-1600 auto fine coater (fig. 8a), the coating
prevents the sample from charging that can occur when the electron bean interacts
with the sample surface, resulting in a better-quality SEM image. Four best samples
were selected based on their colour and yield and observed using JEOL a Jeol SEM
JSM-6701F. The evaluation of the samples were done on the smoothness of the outer
surface of the microencapsules and the particle size.
(a) (b)
Figure 8. (a) Coating the SEM stub with platinum in vacuum (b) scanning electron
microscope (SEM)
12
Project number: SAS-2023-2310-0044
(a)
(b) (c)
Figure 9. (a) electron microscope (b) microencapsulated powder samples placed on the slides
(c) zoomed image of the microencapsulated powder under the light microscope
13
Project number: SAS-2023-2310-0044
METER Aqualab PRE, Benchtop Water Activity Meter was used to measure the water
activity of the samples. The equipment was calibrated using 0.760 water activity
(6.00mol/kg of NaCl in H2O) at 25C. Each of the four samples were placed in the cup
ensuring the surface is fully covered.
14
Project number: SAS-2023-2310-0044
Chapter 3
Results and Discussion
After repeating the experiment several times with changes in different parameters, four
best samples were studied closely to draw a conclusion. The sample were selected based
on the colour of the encapsulated lycopene and relative yield.
15
Project number: SAS-2023-2310-0044
(A) (B)
Figure 13. (A) Sample I (B) sample H2
16
Project number: SAS-2023-2310-0044
41.42% yield where sample F2 was homogenized for 60s after mixing GA,GB and pectin
followed by another 60s after adding the lycopene oil resulting a comparatively higher
yield of 41.81%. Other factors were kept same, results are summarized in the table below.
Temperature Lycopene Alkaline Encapsulation Homogenizing
(°C) oil (g) (w/wo) Yield (%) time (s)
Sample 150 1 w 41.42 GA+pectin, 60s
F1 +GB, 60s
+ lycopene oil,
60s
Sample 150 1 w 41.81 GA+GB+Pectin,
F2 60s
+lycopene oil,
60s
Sample 150 1 w 35.81 GA+GB+pectin,
G1 60s
+ lycopene oil,
120s
Sample 150 1 w 37.41 GA+GB+Pectin,
G2 120s
+lycopene oil,
120s
Sample 150 1 w 39.56 GA+GB+Pectin,
G3 180s
+lycopene oil,
180s
Table 3. Effect of homogenizing time on the yield
The homogenizing time was further increased from sample G1 to G3 keeping the other
parameters same. The yield of sample G1 dropped by 7.7% compared to sample F3.
Further increase of the homogenizing time showed an increase in the yield compared to
sample G1. Define parttern of homogenizing time was not found however, the highest
yield was seen with homogenizing time of 60s after mixing GA+GB+pectin and 60s after
adding lycopene oil.
3.1.3 Effect of adding alkaline solution
The below table shows that adding alkaline to balance the pH of the liquid feed resulted
in lesser yield than compared to the same experiment being conducted with no alkaline
added. No conclusion could be drawn out as not enough tests were conducted.
Temperatur Lycopene Alkaline pH Encapsulation
e (°C) oil (g) (w/wo) Yield (%)
Sample A 150 0.75 w 6.52 33.40
17
Project number: SAS-2023-2310-0044
The microencapsulated lycopene is observed as clumps as the sample were not dried in
an oven prior to SEM analysis to retain is spherical shape. Completely drying the
microencapsulated lycopene could collapse its exterior coating and possible lycopene
leakage.
The narrow size distribution observed in the micrographs indicates a consistent and
reproducible microencapsulation process.
(a) (b)
18
Project number: SAS-2023-2310-0044
(a) (b)
(c)
Figure 15. sample H1 (a) magnification x2000 (b) magnification x250 (c) magnification x1000
(a) (b)
Figure 16. sample H2 (a) magnification x1500 (b) magnification
19
Project number: SAS-2023-2310-0044
(a) (b)
Figure 17. sample I (a) magnification x1500 (b) magnification x250
The results after exposing the microencapsulated lycopene to high temperature (40) and
high humidity (70%) it was observed that samples 3, H2 and I retained their original
color whereas sample H1 faded into pale white. This suggest that sample H1 failed to
maintain its stability and retain the lycopene. There is no enough evidence to confirm
why sample H1 failed the stability test however, the moisture content of sample H1 was
noted to be higher (6.95% moisture content) compared to the other three samples (table
1). The other three samples were able to retain their colour and thus, indicating the
microencapsulated lycopene is stable.
(a)
20
Project number: SAS-2023-2310-0044
(b)
Figure 18. Stability test observation (a) before placing the samples in the stability chamber
(b) after taking the samples from the stability chamber
21
Project number: SAS-2023-2310-0044
Chapter 4
Conclusion
22
Project number: SAS-2023-2310-0044
References
[1] Finotelli, P. V. (2005). MICROENCAPSULATION OF ASCORBIC ACID IN
https://www.researchgate.net/publication/242161841_MICROENCAPSULATION_OF_ASCOR
BIC_ACID_IN_MALTODEXTRIN_AND_CAPSUL_USING_SPRAY-DRYING
[2] Santana, A. A., Kurozawa, L. E., De Oliveira, R. A., & Park, K. J. (2013). Influence of process
conditions on the physicochemical properties of pequi powder produced by spray drying. Drying
https://doi.org/10.1080/07373937.2013.766619
[3] Shu, B., Yu, W., Zhao, Y., & Liu, X. (2006). Study on microencapsulation of lycopene by
https://doi.org/10.1016/j.jfoodeng.2005.05.062
[4] Rock CL, Jacob RA, Bowen PE. Update o biological characteristics of the antioxidant
https://pubmed.ncbi.nlm.nih.gov/8675913/
lycopene by spray drying: Characterization, stability and application of microcapsules. Food and
https://doi.org/10.1016/j.fbp.2011.01.001
[7]Souza, A. L. R., Chávez, D. W. H., Pontes, S. M., Gomes, F. D. S., Cabral, L. M. C., & Tonon,
https://doi.org/10.1016/j.lwt.2018.01.053
23
Project number: SAS-2023-2310-0044
[8]Imran, M., Ghorat, F., Haq, I. U., & Jillani, Q. (2020). Lycopene as a natural antioxidant used
https://www.researchgate.net/publication/348578970_Lycopene_as_a_Natural_Antioxidant_Used
_to_Prevent_Human_Health_Disorders
[9] Islamian, J. P., & Mehrali, H. (2015). Lycopene as a carotenoid provides radioprotectant and
https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4297477/
Silva, J. C. (2018, July 11). What is maltodextrin and is it safe?
https://www.medicalnewstoday.com/articles/322426
[11]Guan, T., Zhang, Z., Li, X., Cui, S., McClements, D. J., Wu, X., Chen, L., Long, J., Jiao, A.,
Qiu, C., & Jin, Z. (2022). Preparation, Characteristics, and Advantages of Plant Protein-Based
https://doi.org/10.3390/foods11111562
https://www.healthkart.com/connect/plant-protein-benefits-for-diabetics/
24