Sembiring Et Al 2025 Fabrication and Characterization of Pectin Chitosan Edible Coatings With A Cosmos Caudatus Leaf
Sembiring Et Al 2025 Fabrication and Characterization of Pectin Chitosan Edible Coatings With A Cosmos Caudatus Leaf
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strength and functional benefits.14 Tomatoes coated with freshener, highlighting its antioxidant and antibacterial proper-
chitosan exhibit lower ethylene production, reduced soluble ties.22
solid concentration, and better retention of total acidity and The aim of this study is to investigate the structural and
vitamin C content.15 Notably, chitosan coating also helps antimicrobial properties of pectin-chitosan edible coatings that
preserve the nutraceutical quality of tomatoes by slowing the are enhanced with the C. caudatus leaf extract.23 Specifically,
degradation of bioactive compounds, such as lycopene and the study focuses on characterizing the surface morphology
phenolics, during storage.15 and crystallinity of the coatings, evaluating their antimicrobial
The integration of antimicrobial agents into edible coatings efficacy, and assessing how varying concentrations of pectin
addresses the challenge of microbial spoilage in perishable and kenikir leaf extracts influence these properties. By
foods.16 Microbial contamination is a major cause of food addressing these objectives, the research seeks to identify the
degradation, leading to spoilage and potential health risks.17 most effective coating formulations that balance structural
stability with antimicrobial effectiveness. Understanding the
Antimicrobial agents can inhibit or kill bacteria, fungi, and
structural characteristics of edible coatings is crucial to
other microorganisms that contribute to food spoilage.18
evaluating their performance. Techniques such as Scanning
Natural extracts, such as those derived from plants, provide a Electron Microscopy (SEM) and X-ray Diffraction (XRD)
sustainable source of antimicrobial compounds.1,19 By provide insights into the surface morphology and crystalline
incorporating such extracts into edible coatings, it is possible properties of the coatings, respectively. These analyses help in
to enhance their protective properties while minimizing the assessing how different formulations impact the coating’s
reliance on synthetic preservatives, aligning with the growing ability to form a uniform barrier and interact with microbial
trend toward natural and ecofriendly food preservation agents. Additionally, evaluation of antimicrobial activity
solutions. through tests against common foodborne pathogens provides
The Cosmos caudatus (C. caudatus) leaf extract, derived from information on the effectiveness of the coatings in preventing
C. caudatus, has shown significant potential as an antibacterial microbial growth. The novelty of this research is the
agent in recent studies.20 This plant extract is rich in bioactive incorporation of the C. caudatus leaf extract in a pectin-
compounds with known antimicrobial properties, which can chitosan matrix; it’s unique due to the bioactive profile,
effectively inhibit the growth of bacteria and fungi. The including anthocyanins, flavonoids, and phenolics, which are
incorporation of the C. caudatus leaf extract into edible not commonly used in similar studies.
coatings could enhance their ability to prevent microbial
contamination and extend the shelf life of coated foods.17 2. MATERIALS AND METHODS
Given the promising antibacterial properties of the C. caudatus The experimental stages of this study include materials,
leaf extract, it represents a valuable addition to the formulation preparation, application, physical-chemical characterization,
of pectin-chitosan coatings. Due to its quercetin content, which and antimicrobial activity, as illustrated in Figure 1.
exhibits anticancer properties, C. caudatus leaves (C. caudatus 2.1. Materials. The materials used for the experiment
Kunth.) have been applied as a complementary therapy for included glacial acetic acid, 96% ethanol, glycerol, and
breast cancer. The primary goal of this application is to chitosan, which were purchased from Sentra Chemical
formulate a nanosuspension containing the C. caudatus leaf Laboratory (Indonesia), and pectin from citrus peel, which
extract with cytotoxic activity against MCF-7 breast cancer was purchased from IR & Co. (Indonesia). C. caudatus leaves
cells.21 Recent studies have explored the potential use of the C. and fully mature tomatoes were collected from the local
caudatus leaf extract (C. caudatus) in edible films as a mouth markets in North Sumatra, Indonesia.
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2.2. Preparation. 2.2.1. C. caudatus Leaf Extraction. Quanta Inspect F scanning electron microscope, operated at 25
Fresh C. caudatus leaves were washed and cut. They were then kV. A thin and continuous layer of gold was deposited on the
dried at 40 °C in an oven for 3 days, followed by pulverizing sample surface before the SEM investigation.
and sieving through a 40 mesh sieve before extraction. The C. 2.4.4. Differential Scanning Calorimetry (DSC) Measure-
caudatus leaves powder was extracted using a direct maceration ments. Thermal analysis was carried out utilizing a differential
method. In detail, as much as 100 g of the C. caudatus leaves scanning calorimeter (DSC) (1 Mettler Toledo) using indium
powder was mixed and soaked in 1 L of ethanol for 24 h at in an ultrahigh purity nitrogen environment (flow rate 50 mL/
room temperature with occasional shaking. All of the extract min) by TA Instruments. In two heating−cooling cycles, 8−10
solutions were then filtered using Whatman No.1 filter paper, mg samples were tested at a 20 °C/min heating/cooling ramp.
and the filtrate was evaporated using a rotary evaporator In the first cycle, film samples were heated to 300 °C at 20 °C/
(Rotavapor R-100, BUCHII) at 40 °C to obtain the dry min and then isothermed for 1 min after being equilibrated at
extract.24 The concentrations of the C. caudatus extract used in 100 °C for 1 min. Film samples were equilibrated at 300 °C
this study (1, 2, and 3 g) are well within the limits of natural and isothermed for 1 min in the second cycle and then cooled
plant extract usage in food applications. The bioactive to 100 °C at 10 °C/min and isothermed for 1 min. Each
compounds, including phenolics and flavonoids, are derived sample had three separate thermal scans, and the average
from plants traditionally consumed in various cuisines, which results were presented. Using information from the results, the
supports their biocompatibility and safety. glass transition temperature (Tg) was calculated.25
2.2.2. Preparation of the Liquid Edible Coating of Pectin, 2.4.5. Viscosity Measurements. The viscosity of the coating
Chitosan, and C. caudatus Extract. The liquid edible coating solution is measured using viscometers with the AMETEK
of pectin, chitosan, and C. caudatus extract was prepared using Brookfield brand, using a No. 4 spindle at 100 rpm. As much as
the mixing method. Briefly, as much as 1.5 g of pectin was 200 mL sample of the solution was measured for 5 min at 20
dissolved in 100 mL of distilled water and stirred at 500 rpm °C. The result is expressed in centipoise (cP).26,27
for 30 min. Then, a chitosan solution (1 g of chitosan dissolved 2.4.6. Weight Loss Determination. The total weight loss
in 10 mL of acetic acid) was added. The mixture was stirred at fruit samples were determined by difference in weight between
500 rpm for 1 h at 80 °C. Next, the C. caudatus leaf extract, in the initial and the final storage time28 by eq 1.
varying amounts of 1, 2, and 3 g, was added to the solution. w w2
The samples were then named PCEC0 (the control sample, total weight loss (%) = 1 × 100
w1 (1)
with no addition of the C. caudatus leaf extract), PCEC1 (1 g
of the C. caudatus leaf extract), PCEC2 (2 g of the C. caudatus where w1 is the initial weight at day 0 and w2 is the final weight
leaf extract), and PCEC3 (3 g of the C. caudatus leaf extract). at the end of storage studies. The experiment was performed
After cooling for 30 min, 1.5 mL of glycerol was added to each independently in triplicates.
variation of the mixture, and it was stirred for an additional 30 2.5. Antimicrobial Activity. In vitro antimicrobial activity
min. was measured by using the disk diffusion method. Bacterial
2.3. Application in Tomato Coating. The tomatoes were suspensions (108 CFU/mL) of Staphylococcus aureus and
selected based on uniformity in size, maturity (mature red), Pseudomonas aeruginosa were swabbed into solidified Mueller−
and absence of external damage. They were washed with Hinton agar. After 5 min, the 6 mm cut PGTC films were
running water and dried naturally at room temperature. placed on top of solidified agar in 9 cm Petri dishes. The Petri
Afterward, they were dipped into edible coating solutions for dishes were incubated at 37 °C for 24 h in an incubator. Using
one min, and tomato without edible coating was used as the a caliper, we determined the inhibition zones of the
control in the experiment. The coated tomato samples were nanocomposite films. The index of antimicrobial activity can
stored at room temperature for 21 days, and weight loss was be calculated using eq 2.
observed.
2.4. Physical-Chemical Characterization of the Liquid index of antimicrobial activity (mm)
Edible Coating of Pectin, Chitosan, and C. caudatus diameter of inhibition zone diameter of film (6 mm)
Extract. The sample was pressed into a solid form on a glass =
diameter of film (6 mm)
slide before being measured with FT-IR spectroscopy, powder
(2)
X-ray diffraction (XRD), morphology measurement, and
differential scanning calorimetry (DSC) analyses. In addition
to these analyses, viscosity and weight loss measurements were 3. RESULTS AND DISCUSSION
also conducted. 3.1. FT-IR Analysis. FT-IR analysis was conducted to
2.4.1. FT-IR Spectroscopy. Fourier transform infrared (FT- determine the components present in the liquid edible coating
IR) spectra were recorded using an IR spectrometer (Jasco layer, both without and with the addition of the C. caudatus
FT/IR 200, Japan) with an infrared microscope with an ATR- leaf extract. In Figure 2, the control sample (PCEC0) shows a
1000-VS objective. The spectra were obtained as the average of sharp peak at a wavelength of 3307.06 cm−1, indicating the
50 scans recorded at a resolution of 4 cm−1 in the range from absorption of the −OH group, specifically phenol. Similarly, a
4000 to 500 cm−1 with a DLATGS detector. medium peak at 1594.66 cm−1 corresponds to the absorption
2.4.2. X-ray Powder Diffraction (XRD) Measurements. A of the aromatic C�C group. Peaks at wavelengths of 1029.69
Shimadzu XRD 7000 diffractometer with Ni filtered Cu Kα and 1108.05 cm−1 indicate the absorption of the C−O group,
radiation (λ = 1.5406 Å), 2θ ranging between 10 and 80°, was which aligns with the functional groups found in pectin and
used for the compositional and structural characterization of chitosan.
the samples through X-ray diffraction (XRD). The graphs for the PCEC1, PCEC2, and PCEC3
2.4.3. Morphological Measurements. Microscopic mor- compositions, shown in Figure 2, indicate that anthocyanin
phology of obtained dried coatings was explored by using a FEI compounds from the C. caudatus leaf extract are bound to the
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Figure 4. SEM images of (a) pectin-chitosan (1000 times magnification), (b) pectin-chitosan with the C. caudatus extract (1000 times
magnification), (c) pectin-chitosan (5000 times magnification), and (d) pectin-chitosan with the C. caudatus extract (5000 times magnification).
Table 2. Weight Loss Percentage of Tomatoes Stored for 7, edible and biodegradable, the residue does not pose significant
14, and 21 Days health risks.
weight loss over weight loss over weight loss over
sample code 7 days (%) 14 days (%) 21 days (%) 4. CONCLUSIONS
without an 8.84 ± 0.29 16.64 ± 0.38 27.55 ± 0.19 This study successfully developed pectin-chitosan edible films
edible coating
PCEC0 6.04 ± 0.09 7.01 ± 0.12 7.84 ± 0.20
enhanced with the C. caudatus leaf extract, demonstrating
PCEC1 5.42 ± 0.15 6.2 ± 0.10 7.51 ± 0.14 improved antibacterial properties. The addition of the C.
PCEC2 5.35 ± 0.22 6.53 ± 0.13 7.03 ± 0.13 caudatus leaf extract to pectin-chitosan coatings significantly
PCEC3 4.06 ± 0.06 5.24 ± 0.29 6.18 ± 0.19 enhanced the preservation qualities of tomatoes by reducing
weight loss during storage and increasing the antibacterial
7 days, 7.01% after 14 days, and 7.84% after 21 days. The activity. The integration of bioactive compounds, such as
addition of the C. caudatus leaf extract further reduced the anthocyanins, into the coating matrix contributed to these
weight loss percentage. A higher concentration of the C. improvements, making the developed coatings a promising
caudatus leaf resulted in a lower weight loss percentage, with option for extending the shelf life of tomatoes. The enhanced
the lowest weight loss observed for PCEC3 samples: 4.06% antibacterial effects, particularly against E. coli and S. aureus,
after 7 days, 5.24% after 14 days, and 6.18% after 21 days. This underscore the potential of these coatings for safe and effective
indicates that the edible coating with the addition of the C. food preservation applications.
caudatus leaf extract can slow down respiration and
transpiration rates, which is related to the antibacterial
properties of the extract, thereby providing optimal protection
for tomatoes during storage and maintaining their quality for
■ ASSOCIATED CONTENT
Data Availability Statement
longer.37 The data that support the findings of this study are available on
3.7. Antibacterial Activity Analysis. Measuring anti- request from the corresponding author.
bacterial activity is a crucial aspect of evaluating edible
coatings. Antibacterial properties in a coating can help slow the
decay process caused by bacterial growth. By comparing the
antibacterial activity of pure pectin-chitosan samples with those
■ AUTHOR INFORMATION
Corresponding Author
containing the C. caudatus leaf extract, the impact of the extract Erna Frida − Post Graduate Program (Physics), Faculty of
can be effectively analyzed. Table 3 presents the results of Mathematics and Natural Sciences, Universitas Sumatera
Utara, Medan 20222, Indonesia; Phone: +62 812-6357-
Table 3. Results of Antimicrobial Analysis 0509; Email: [email protected]
zone of inhibition (mm) Authors
sample code E. coli S. aureus Emita Sembiring − Post Graduate Program (Physics), Faculty
PCEC0 11.32 ± 0.1 10.21 ± 0.1 of Mathematics and Natural Sciences, Universitas Sumatera
PCEC1 13.4 ± 0.1 12.83 ± 0.1 Utara, Medan 20222, Indonesia; orcid.org/0009-0002-
PCEC2 13.96 ± 0.1 13.47 ± 0.1 5263-3347
PCEC3 14.06 ± 0.1 15.23 ± 0.2 Zuriah Sitorus − Post Graduate Program (Physics), Faculty of
Mathematics and Natural Sciences, Universitas Sumatera
Utara, Medan 20222, Indonesia
measuring the diameter of the inhibition zones for Escherichia Timbangen Sembiring − Post Graduate Program (Physics),
coli and S. aureus bacteria in the samples. The PCEC0 sample Faculty of Mathematics and Natural Sciences, Universitas
produced an inhibition zone of 11.32 mm for E. coli and 10.21 Sumatera Utara, Medan 20222, Indonesia
mm for S. aureus. The addition of the C. caudatus leaf extract Complete contact information is available at:
enhanced the inhibition zones for E. coli, increasing to 13.40, https://pubs.acs.org/10.1021/acsomega.4c10344
13.96, and 14.06 mm for PCEC1, PCEC2, and PCEC3,
respectively. Similarly, the inhibition zones for S. aureus Author Contributions
increased to 12.83 mm (PCEC1), 13.47 mm (PCEC2), and E.S.: Conceptualization, methodology, validation, formal
15.23 mm (PCEC3). These results indicate strong antibacterial
analysis, investigation, writing�original draft. E.F.: Method-
activity, as inhibition zones larger than 11 mm are classified as
strong, while those smaller than 6 mm are considered weak.38 ology, resources, formal analysis, investigation, writing�
In general, this study shows that the increase in the review, editing, supervision. Z.S.: Investigation, conceptualiza-
concentration of the C. caudatus leaf extract in the edible tion, methodology, formal analysis, resource. T.S.: Formal
coating is directly proportional to the increase in the diameter analysis, term, validation.
of the inhibition zone, which identifies a fairly antibacterial Notes
solid effect. This is due to the high content of bioactive The authors declare no competing financial interest.
compounds, specifically polyphenols and flavonoids, in C.
caudatus leaves, which have antibacterial and antioxidant
properties.20 The C. caudatus extract is nontoxic and safe for
consumption; however, to mitigate residue concerns, it is
■ ACKNOWLEDGMENTS
The authors are grateful for Post Graduate Program Depart-
recommended that a lightly rinse-coated product be consumed ment of Physics, Faculty of Mathematics and Natural Sciences,
before consumption. Additionally, given that this coating is Universitas Sumatera Utara.
7209 https://doi.org/10.1021/acsomega.4c10344
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