Redo Indicator Label in Potato Starch Film as Fruits Quality Monitoring (Case:

Strawberry fruit)
Soffi Syarofah#, Zainal Alim Mas’ud#, Henny Purwaningsih*
# Department of Chemistry, Bogor Agricultural University, Ge dung Kimia Wing 1
Lanai 3, Jalan Tanjung
Campus IPB, Bogor, 16680, Indonesia
E-mail: soffi_syarofah@apps.ipb.ac.id
#Laboratories Terpadu, Campus IPB Baranangsiang Wing Kimia, Lanai Dasar, Kota
Bogor, 16144, Indonesia
E-mail: zainallim@yahoo.com
#Department of Chemistry, Bogor Agricultural University, Ge dung Kimia Wing 1
Lanai 3, Jalan Tanjung
Campus IPB, Bogor, 16680, Indonesia
E-mail: hennypurwaningsih@gmail.com

Abstract— The film indicator label is one of smart packaging that can be used
monitoring fruit damage. The label indicator detects volatile compounds produced
by the fruit ripening process based on the oxidation-reduction reaction. In this
study, we used potato starch as a film matrix, iodine as a color indicator, and
paraffin as a protector against moisture of film surface. The indicator label
has been made by mixing potato starch and iodine solution in various
concentrations. Further treatment on the label was carried out by coating
method. All indicator label samples were used in packaged fruits and kept in
room temperature (25 oC) and chill temperature (14 oC). The change in color
intensity on the indicator labels were measured using by UV-Visible
Spectrophotometer (UV-Vis), the characteristics of the film were analyzed using
by infrared spectroscopy (FTIR), and simulations of ethylene gas were also
carried out to test the amount of ethylene concentration on the indicator label.
This result is supported by a decrease in UV-Vis spectra during the observation
period at wavelengths of 475 nm and 316 nm with almost linear curves. The
infrared spectra also show the iodine wave number is missing after application
on fruit. Thus, the results show that this indicator label made with a mixture
of starch and iodine can be applied as an indicator that is easy to use and
promises to monitor damage packaging fruits.

Keywords— indicator label, smart packaging, fruits quality monitoring, iodine,

potato starch, ethylene.

I. Introduction
Strawberry fruit (Fragaria×Ananassa) is a berry plant worldwide that is most
often consumed because it is rich in nutrients and its unique taste [1].
However, strawberries are easily spoiled during transportation and storage, thus
causing significant economic losses [2]. In Indonesia, the contribution of
strawberry production to 58882 tons / ha has dropped dramatically by 34.7%,
compared to 2012 [3]. According to Kader et al. [4], consumers experience
difficulties in knowing the level of freshness of fruit when on the market. It
is important to minimize physical damage to fresh fruit products to obtain
optimal shelf life. The use of packaging is a suitable solution [5]. Packaging
has an important role in the food industry because they act as inhibitors of the
factors responsible for damage to chemicals, physical and microbiological
materials in food.
Smart packaging is a packaging innovation that aims to help consumers know the
freshness of a product. In Indonesia, starch-based packaging applications that
can be decomposed in fresh products have been studied and evaluated for some
time. Some authors conclude that they can be used to package food with low water
activity [6, 7]. Warsiki et al. [8] has developed a color indicator label for
ammonium molybdate to detect the maturity of climacteric fruit based on the
presence of ethylene gas due to the process of respiration. Likewise, Kuswandi
[9] has developed a blue bromophenol membrane to detect the freshness of guava
fruit based on a decrease in pH. Fantastic [10], has developed an indicator
label to detect the level of freshness of non-climacteric fruit in the presence
of volatile acid gases and CO2 packaged in fruit. However, the development of
this packaging is less attractive to be applied commercially due to several
factors such as unclear licensing regulations, and packaging costs that do not
seem to reduce production costs [11]. Non-renewable sources of polymers that
have been used in many packaging applications because they are durable, durable,
easy to process and low cost. However, this kind of material usually carries
serious problems with the environment due to decomposition difficulties [12].
One alternative to reduce environmental impact is biodegradable packaging
obtained from renewable sources such as starch and cellulose [13, 14]. The use
of starch as a supporting medium (matrix) in packaging materials has been
studied because of the nature of biodegradability, low total costs, and
availability throughout the world [15, 16]. Potato starch is one of starch which
provides better film formation properties than other films [17]. Films with the
highest amylase content generally have more resistant mechanical properties.
However, the use of potato starch (PS) with 80% amylopectin has several
disadvantages in low humidity sensitivity, poor mechanical properties, and poor
solubility [18]. The use of a coating method or deposition of a thin layer of
surface to improve the waterproof properties of good packaging interests [19].
Thus, to minimize water absorption by starch foam, Ba ratter [20] reported the
application of hydrophobic coating or impregnation. Many ingredients have been
studied, one of which is Paraffin. This is because paraffin has properties that
can improve water resistance to cellulose polymers.
The selection of color indicators based on acid-base reactions in the fruit
ripening process has not been widely studied. Based on this information, the
color indicator that is suitable and easy to use is using iodine. Iodine can be
homogeneous with starch and can interact with ripening gas (ethylene). Ethylene
is able to show significant color changes to the indicator label during the
ripening time to decay. This phenomenon results in discoloration of labels that
were originally solid purple to colorless. The purpose of this study is to
develop a label for film indicators with a matrix of potato starch based on
redox phenomena so that they are easy to use for consumers and promising for the
packaging industry in monitoring the damage to packaging fruit.
II. Materials and Methods
A. Materials
Strawberry was purchased from the local market of Bogor, Indonesia. The
chemicals used in this study were potato starch (5% v/v), iodine (Merck, DE),
potassium iodide (Merck, DE), distilled water, hexane (Merck, DE), and paraffin
(Merck, DE) (5% v/v).
B. Methods
1) Color indicator solution preparation: The color indicator consists of iodine
(I2) and potassium iodide (KI) with two variations of concentration A (0.015%
(v/v) I2, 0.15% (v/v) KI) and concentration B (0.010% (v/v) I2, 0.1% (v/v) KI).
2) Indicator film preparation by casting method: potato starch 5% (v/v) was
prepared with 8 formulations. The casting method is used to produce films by
printing formulation solutions on an acrylic plate. The film are given two types
of treatment, Further treatment on label was carried out by coating method with
paraffin. All indicator label sample were used in packaged fruits and kept in
room temperature (24 oC) and chill temperature (14 oC). (Table 1) showing the
formula code based on treatment. The selection of the best formulation is based
on the physical properties of the label which includes the level of
discoloration observed visually and the effectiveness of the indicator label
when applied.
TABLE I
Indicator film formulation
Code
Formula

[I3-] (%)
Color indicator (mL)
Starch (%v/v)
Distilled water (mL)
Temp. (oC)
Treatment
B
0.1
7.5
5
50
24
non coating
C
0.1
5
5
50
14
coating
D
0.1
7.5
5
50
24
non coating
E
0.1
5
5
50
14
coating
F
0.75
7.5
5
50
24
non coating
G
0.75
5
5
50
14
coating
H
0.75
7.5
5
50
24
non coating
I
0.75
5
5
50
14
coating

The process of stirring a potato starch solution 5% (v/v) was carried out using
a magnetic stirrer hotplate for 20 minutes at a temperature of 70 oC to form a
gel or film solution [21]. Storage for 15 minutes at room temperature is done to
eliminate the effects of the heating process. After that, the film solution is
added to the color indicator during the stirring process for 1.5 hours and is
left to stand for 2 hours to remove foam due to the stirring process. Film
solutions that have been homogenized with color indicators are printed on
acrylic plates using a casting method, then dried for 20 hours at temperature 21
± 2 oC and relative humidity (RH) 65 ± 5%. Films manufactured were peeled and
cutting into circle of 2 cm in diameter pieces, thus forming an indicator label.
3) Film coating: paraffin 5% (v/v) is dissolved with hexane as much as 50 mL
until it is homogeneous. The indicator label that has been made is then coated
with a 10% (v/v) paraffin solution with the dipping method and dried for 2 hours
at room temperature.
4) Application on fruit: The prepared strawberries are packed using a plastic
wrap that has been affixed with a polymeric indicator on a Petra dish with a
different temperature treatment. Container A at 24 ºC (room temperature) and B
at 14 ºC. Indicator color changes that occur are observed periodically (per
day).
C. Characterization
1) UV-Vis spectroscopy: Analysis using the Ocean Optic USB 4000 devices with a
wavelength of 250-600 nm.
2) Fourier Transform Infrared (FTIR): FTIR analysis (Perkin Elmer FT-IR
Spectrometer Spectrum One) aims to identify the characteristics of PS films with
iodine indicators before and after application of fruit. Analysis of samples
with FTIR was carried out at a resolution of 4.00 cm-1 and payar 32.

III. Results and Discussion

A. Synthesis of film indicator labels
1) Formula label indicator films
Potato starch (PS) was chosen as the base material for making indicator films
because PS can form films that have a uniform and smooth surface [22]. The
selected color indicator is iodine, because iodine in a starch solution
establishes a helical chain with a configuration bond in each glucose unit. This
form causes starch to form complexes with iodine molecules that can enter into
the spirals, causing a dark blue color in the complex.
PS reacts with iodine molecules because the structure of the starch in a helical
solution is in the form of a coil so that it can be filled with iodine molecules
in it. However, after reacting with fruit ripening gas, the color of the
indicator label becomes colorless. This is due to the termination of iodine
bonds due to interacting with ethylene. Making the film label indicator is based
on a redox reaction that indicates a change in color on the indicator label
(Reaction 1 & Reaction 2).
Reaction 1:
I2 + I-  I3- + starch
0 -1
reduction
(amber) (dark blue complex)

Reaction 2:
starch + 2I3- + 3C2H4  3C2H4I2
-1 0 0
oxidation
(colorless)
The formula is divided into 8 letter codes (Table 1). Formula B is the formula
that experiences the most stable color changes. Based on Harris [23],
strawberries have rotten after 4 days of ripening process. As for the other
formulas, when the fruit is not rotten, the color on the label has faded or the
color on the label remains intact but the fruit is rotten, so the other formula
cannot be used. Iod is a compound that is very sensitive to light and air so
coating is needed to the physical condition of the film remains strong. The
coating is done by adding paraffin to the film so that the film is not easily
vulnerable when exposed to moisture. According to Billmayer [24], paraffin has
properties that can improve water resistance to cellulose polymers.
2) Color indicators are made by dissolving iodine (I2) and potassium iodide (KI)
solutions. The addition of KI is intended to increase its solubility, thus
forming polyodide ions namely I3–. The negatively charged iodide in this
compound acts as a charge donor, neutral iodine as a charge accept or. Electrons
in the complex transfer such charges easily aroused (excited) to higher energy
levels by light, resulting in dark orange-brown colors [25].
3) Synthesis of film
Starch consists of two types of polysaccharides namely amylase (linear) and
amylopectin (branching). Potato starch contains 20.02% to 21.59% in starch
granules [26]. Starch-iodine forms another charge transfer complex, with the
amylase chain binding to iodine to form a helix. Amylose acts as a charge donor
and polyodide as an accept or. This complex absorbs light with different
wavelengths of polyodide, and the color changes to deep blue or purple-black.
Iodine in amylase produces blue-black, while iodine in amylopectin forms a
reddish-brown or purple solution. Because amylopectin is highly branched, it
only binds a small amount of iodine and produces a pale purple-red color.
4) Polymeric indicator label
The polymeric indicator label is made by dissolving the starch solution and
adding an I3- color indicator, then stirring using a magnetic stirrer for 1.5
hours at room temperature. After that, let stand for 2 hours to remove bubbles
due to the process of stirring. The film solution was then printed on a 15 × 10
cm acrylic board using the casting method and dried in a room with 65% humidity
(21 oC) for 20 hours. The dried film is then released and a circle with a
diameter of 2 cm is released. Coating on the film is done to protect indicators
that are sensitive to light and improve the physical properties of the film.
Fig. 1 Polymeric film indicator label based on variation of formula
5) UV-Vis Spectroscopy Analysis
Changes in the color intensity on the selected indicator label (sample B) were
analyzed to see the effectiveness of iodine as a color indicator. Fig. 2a shows
that the film undergoes discoloration from deep purple (before application) on
day 0 becomes colorless (after application) on day 5 (Fig. 4). The color of the
label tends to change from day 2 at room temperature and day 3 at cold
temperatures. The color change is marked at a maximum absorption peak of 475 nm.
The calibration curve shows the value of the ratio of absorbance at 475 nm (y =
-0.2379x + 2.0522) and at 316 nm (y = -0.1377x + 1.3597) at room temperature.
Whereas in cold temperatures the absorbance ratio is 475 nm (y = -0.1293x +
1.5229) and at 316 nm (y = -0.1085x + 1.1235). The formula shows the exponential
function with the coefficient determination (R2) which is almost close to 1
(Fig. 3). The results showed that the number of blue compounds in the film
indicator label experienced a significant color change. Lambert's Law which
states that the concentration of the color compound in a solution is
proportional to the absorbance in the wavelength at which it absorbs [27]. Based
on the data that has been obtained, I3- has the potential for use as a color
indicator for labels, because of the sensitivity that changes the color from
blue to colorless.

6) FTIR Analysis aims to identify molecular interactions between component of

indicator film labels at wave number of 400–4000 cm-1 (Fig. 4). The selected
film indicator label based on the UV-Vis result is sample B, with the most
stable color change. Characteristic peaks at wave number 3248 cm-1 (stretch O–
H), this is similar to the results reported by Kumar et al. [28], Byun &
Yoon [29], and Sharma et al. [30]. In the band 2922–2918 cm-1 shows the C–H
aromatic group [31]. The interaction between starch and hydrogen bonds (starch
hydration) is shown as a characterization peak with a wave number 1640 cm-1,
which is a stretch of C=O (carbonyl) in the ester group in modified (film)
starch [32]. The reactions that occur during the process of forming the film
cause visibility of the ester group (esterification reaction) [33].
Characteristic peaks in the range 1000–1400 cm-1 are stretches in the glycosidic
bonds [34].
Singh et al. [35] state that the characterization peak at wave numbers around
1000 cm-1 is recognized as a water sensitive area and is associated with
hydroxyl group intramuscular hydrogen bonds or the effects of water
platinization.The characteristic peak of the iodine group (C–I), shown in wave
number 611 to 528 cm-1 before treatment (above). According to Silverstein [36]
(1997) regions with wave numbers 690-515 cm-1 are alkyd halides, namely
compounds that have C–-X bonds, with X being halogens such as bromine, chlorine,
fluorine, or iodine. Singh et al. [35] stated that FTIR is a short-term analysis
technique used to infer crystallinity. The peak of the iodine group after
treatment showed widening, this was due to the interaction between iodine groups
and fruit ripening gases (Reaction 2). The shape and width of the peak only
identify the nature of the vibration and the spread of the vibration frequency,
so that the intensity and position of the peak are indicative of the level of
order and in the conformation system.

7) Sensitivity test
The sensitivity of the film indicator label was measured using two application
techniques: a) the technique of exposure to gas maturation directly on
strawberries; and b) the technique of injecting ethylene gas into a bottle with
a modified device (Fig. 9).
 a) Applications on fruit: a) Application on fruit: Changing the color of an
indicator label has occurred in the results of exposure using strawberry fruit.
In this technique, ethylene is emitted from strawberries (Fig. 5). The fresh
strawberry washed with alcohol to remove bacteria or dirt attached to the fruit,
then strawberries were given two storage temperature treatments, namely at 24 oC
and 14 oC. Two strawberries are placed on Petra dish, then packaged in a plastic
wrap that has been labeled with an indicator. Color changes in indicator labels
and fruit damage are observed every day (Fig. 6). Indicator labels have been
exposed to ripening gas from strawberries were then analyzed using UV-Vis (Fig.
2).
According to Perangin-angin [37], in fruit ripening, ethylene degrades the
chlorophyll in immature fruit, so the fruit has only xantofil and carotene.
Ethylene will be emitted from the entire surface of the fruit due to the
metabolic process that begins with protein synthesis at the level of normal
maturation. Furthermore, the metabolic processes occurring in fruit that cause
qualitative changes in respiration rate.

b) Applications on ethylene gas: In sensitivity testing, ethylene gas 99% were

carried out with two treatments are time and pressure variations (Fig. 9).
Concentration of ethylene gas will affect changes in indicator labels. Ethylene
gas is flows from the gas cylinder through a modified gas appliance, then flows
into a glass bottle that has an indicator label.

Ethylene gas is flows at a pressure of 0.57 atm (50 cmHg), and then all valves
are closed to ethylene gas to spread evenly and interact with the indicator
label. The film matrix which has high permeability will pass ethylene gas
interacting with the color indicator (iodine). The first treatment was carried
out several time variations, are 2, 4, 6, 8, and 10 hours. After observation,
the indicator label does not show color change again at 6 hours. This data is
supported by UV-Vis which shows the range of absorbance values (Fig. 7).
Furthermore, several gas pressure treatments were carried out, namely 0.13,
0.26, 0.39, 0.53 and 0.57 atm with the exposure time of ethylene gas for 6
hours. After observation, UV-Vis analysis was performed to produce a correlation
curve between pressure (x) and concentration (y). The curve states that the
pressure is directly proportional to the amount of the concentration of ethylene
gas with a value with R2 = 0.9741 at a wavelength of 485 nm (Fig. 8). The
greater the ethylene gas pressure is given, the greater the amount of gas
concentration produced. The amount of ethylene concentration can be known
through equations:
PV = nRT
With:
P= Pressure (atm) n = mol of gas (mol)
V= bottle volume (L) R= 0.082 L atm/mol. K
T= temperature (K)

The mechanism of discoloration caused by ethylene chemical reactions has not

been fully known and studied [38]. In this study, the label indicator uses the
phenomenon of oxidation-reduction reactions to detect the presence of ethylene
(Reaction 2). As a result of the interaction between ethylene gas and the label
indicator, this causes the color indicator that was originally purple-black to
turn colorless.
 IV. Conclusions
Indicator labels have been successfully applied to strawberries and show color
label changes along with fruit quality. Coating using paraffin successfully
improves the physical properties of the film without changing the color of the
indicator. UV-VIs analysis which showed a decrease that occurred during the 5
days of observation. FTIR analysis also shows that groups (C — I) have been lost
when applying to fruit. The gas simulation results using ethylene gas after UV-
Vis analysis on the curve of comparison between pressure (x) and absorbance (y),
obtained the coefficient determination at a wavelength of 485 nm. This proves
that the indicator label of this film is feasible in the packaging industry with
efficient production costs and can facilitate consumers in monitoring damage to
fresh fruit.

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