Antibacterial Performance of Tencel Fabric Dyed With Pomegranate Peel Extracted Via Ultrasonic Method
Antibacterial Performance of Tencel Fabric Dyed With Pomegranate Peel Extracted Via Ultrasonic Method
https://doi.org/10.1007/s10570-018-1864-6
ORIGINAL PAPER
Received: 14 January 2018 / Accepted: 21 May 2018 / Published online: 24 May 2018
Ó Springer Science+Business Media B.V., part of Springer Nature 2018
Abstract Application of naturally dyed fabrics is dyeing. Dyed samples were analyzed with rubbing,
increasing due to the biological protection, pollution washing, perspiration and light exposure tests for color
control, ecology and improved quality of life of human fastness. The results revealed that different types of
beings. Antimicrobial textiles can be the best choice to mordants have dissimilar effects on color efficiency and
avoid fabric related infection. Many plants have been color range values of dyed lyocell fabrics. The dyed
regarded as suitable for extraction of natural dyes that fabric with different mordants showed excellent color
can also show good antibacterial activity. However, in strength (K/S) values (6.4) and color fastness properties
this work, natural dye from pomegranate peel was of washing (4–5), light (5–6), rubbing (4–5) and
extracted by ultrasonic method and then lyocell fabrics perspiration (4–5). Furthermore, FTIR confirmed that
were treated with different mordanting agents. After- no structural change occurred in the lyocell fabric before
wards, mordanted fabric samples were dyed by exhaust and after the dyeing process. Additionally, antimicrobial
properties of un-dyed and dyed with pomegranate peel
were assessed against Staphylococcus aureus (ATCCÒ
F. Rehman Y. Wang W. Wei (&) 25923TM) by the agar diffusion test method. The
College of Chemistry, Chemical Engineering and obtained antimicrobial activities of the samples dyed
Biotechnology, Donghua University, Shanghai 201620, with pomegranate peel were compared with that of the
China
un-dyed samples. The un-dyed samples displayed slight
e-mail: [email protected]
antibacterial properties while fabrics dyed with pome-
N. Sanbhal granate peel exhibited suitable antibacterial properties.
Department of Textile Engineering, Mehran University of Thus, lyocell fabrics dyed with pomegranate peel are
Engineering and Technology, Jamshoro, Sindh 76060,
useful for biomedical applications.
Pakistan
T. Naveed
School of Fine Arts, Design and Architecture, GIFT
University, Gujranwala, Pakistan Introduction
W. Wei
Saintyear Holding Group Co., Ltd., Since ancient times, illnesses and infections are major
Xiaoshan, Hangzhou 311221, Zhejiang, China concerns for people and safety authorities (Gupta et al.
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4252 Cellulose (2018) 25:4251–4260
2004). Therefore, pomegranate has been added as an presence of tannins, anthraquinones, naphthoquinones
antibiotic in medicines, preservatives and textiles to etc (Lee et al. 2009). The pomegranate peel has been
increase the safety and protection of human life (Onar reported as an antimicrobial agent that contains a
et al. 2011). Furthermore, pomegranate peel has significant amount of phenolic compounds, tannin
diverse biological functions that prevent various (approximately 19%), with pelletierine (Prashanth
illnesses and subsequently can impart antimicrobial et al. 2001). Therefore, the fabrics dyed with
properties to the textiles (Negi and Jayaprakasha pomegranate peel have the influence of an anti-allergic
2003). Thus, antimicrobial textiles have been consid- and antibacterial property (Malviya et al. 2014).
ered to be the best choice for clinical and medical There are many readings on antimicrobial textiles
applications to reduce the transmission of infection (Adhami et al. 2009) despite the fact, no studies have
produced by bacteria (Sun 2011). However, the been described in the literature regarding antimicro-
majority of the infections concerned in hospitals are bial lyocell fabrics using pomegranate peel. Although,
due to S. aureus (SA) (Sanbhal et al. 2018a). As a lyocell fabrics have been dyed with synthetic (reac-
consequence of the growing concern about health and tive) dyes and variety of colors, light to dark were
the environment, clothing that comes in contact with produced (Babar et al. 2017) but the main drawback of
the human skin is preferred to be non-toxic (Simoncic reactive dyes is that it does not exhibit antimicrobial
and Tomsic 2010). Therefore, in recent years tendency functions. Thus, pomegranate peel dyed fabrics with
towards the evaluation of microbial attack on textiles antimicrobial properties could be a good replacement
and their prevention measures has been increased (Al- of reactive dyed lyocell fabrics. Pomegranate peel
Zoreky 2009). Thus, antimicrobial textiles have been a contains granatonine, the main coloring agent present
basic necessity for avoiding skin infections (Ismail in the form of N-methyl granatonine (Kulkarni et al.
et al. 2012; Kim et al. 2002). 2011). This eco-friendly compound provides color to
Antimicrobial properties on textiles are achieved by the dye (Adeel et al. 2009). However, it has low
physical or chemical incorporation of antibacterial exhaustion and poor fastness properties on textile
agents. The chemically incorporation of antimicrobial fabrics without mordants (metallic salts) (Goodarzian
agents onto the fabrics is interacts through strong and Ekrami 2010). The pomegranate extracted dye has
intermolecular interactions such as covalent or ionic been explored for its potential antimicrobial properties
connections between fibers and the antimicrobial against common bacteria, such as S. aureus and
agents depending on the structures of fibers and fixing Escherichia coli (Lansky and Newman 2007).
agents. Thus, antimicrobial such as quaternary ammo- In this present investigation, pomegranate peel was
niums salts phenols and halamines as well as some extracted by using suitable ultrasonic method. The
inorganic compounds based on silver and copper ions extracted antimicrobial dye was applied on lyocell
are commonly used. However, the main disadvantage fabrics by exhaust dyeing technique. The resultant
of these chemicals containing antibiotics has environ- dyed fabrics were characterized using Fourier Trans-
mental issues (Sun 2011). form Infrared Spectroscopy (FTIR) and different
Antibacterial natural dyes have gained an impor- colorfastness tests. Furthermore, the colorimetric
tance for utilization as antimicrobial substances. The parameters i.e. color strength (K/S) value and the
use of antimicrobial compounds specifically from the Hunter coordinate (L*, a*, b*) values of dyed samples
natural sources (Ibrahim et al. 2010; Singh et al. 2005) for color depth have been examined in this work. The
including pomegranate polyphenols are present and dye absorption (%) and the color fastness properties of
can demonstrate suitable antimicrobial activity (Mah- the dyed fabric have also been evaluated for their
mood et al. 2010). The literature reviewed shows that durability. Moreover, antibiotic properties of control
natural dyes are used not only to provide color but also and pomegranate peel dyed fabrics with and without
improve antibiotic resistance to the microbial growth mordants were conducted using agar diffusion test
(Prusty et al. 2010). These dyes are effective due to the method.
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Cellulose (2018) 25:4251–4260 4253
Experimental work samples were used for dyeing. Table 1 shows the
recipe of mordanting process.
Materials and methods
Dyeing
Pre-treated (white) 100% lyocell fabric was obtained
from Hangzhou Xinsheng printing and dyeing Co., Dyeing was performed with and without chemicals
Ltd., China. The lyocell fabric with plain weaved (mordanting agents) to examine the dyeability of
(warp-30, weft-30, fabric density 128 9 82 and fabric lyocell fabrics. Thus, 2.5 g of fabrics containing 7 mL
weight 160 g/m2) was selected for pomegranate peel of dye solution was kept in all beakers of 100 mL.
dyeing. Pomegranate Peel (Punica granatum) was These beakers were loaded in a shaker dyeing machine
obtained from a domestic market of Shanghai. Son- for 1 h at 90 °C temperature. The material to liquor
icator bath was used for the extraction of the natural ratio was kept 1:40. After dyeing process soaping of
dye from pomegranate peel. All experiments of dyeing dyed lyocell fabrics were performed to remove
and mordanting were performed by using water unfixed surface dyes. Soaping process was consisted
shaking dyeing machine (made in China). Laboratory of five washing cycles for at least 10 min of contin-
grade metallic salts such as ferrous (II) sulfate uous washing. 1st cold wash (normal room tempera-
(FeSO47H2O), copper (II) sulfate (CuSO45H2O), ture), 2nd hot wash (70 °C), 3rd hot wash (70 °C) with
tin (II) chloride (SnCl22H2O), Alum (KAl (SO4)2- soaping agent, 4th hot wash (70 °C) to remove soaping
12H2O), and potassium dichromate (K2Cr2O7) man- agent and finally cold rinse at room temperature.
ufactured by Sinopharm Chemical Reagent, Co., Ltd.) All washed samples were dried at room temperature
were selected as a mordants. The industrial soaping for 24 h. Moreover, 2 g/l of industrial soap was used
agent was received from Hangzhou Xinsheng printing as a soaping agent for all dyed samples. The dyeing
and dyeing Co. Ltd., China, for soaping process. recipe and process parameters are shown in Table 1.
The ultrasound-assisted extraction method was used CIE L*a*b* values were used to measure the range of
for the extraction of dye from the pomegranate peel. colors on to dyed lyocell fabrics. Spectra Flash-Data
10 g powder of pomegranate peel was placed in the Color (SF-600) was used to measure the values and
beaker and 200 mL solvent (120 mL ethanol and also dye absorption properties on the fabric surfaces.
80 mL distilled water) was added with material to CIE L*, a*, b* is a color space standard, identified by
liquor ratio 1:20. The beakers were then placed in the the international commission on illumination. The L*
ultrasonic bath and sonicated for 1 h at 50 °C value indicates the brightness and its values ranges
temperature with frequency 27–30 MHz and 160 V from 0 to 100. It describes that higher value of L* has
supplied. Subsequently, the solutions were filtered lighter shades and lower value of L* has darker shades
through Whatman filter paper and solvents were for the lyocell fabric. The ? a* value shows red and
evaporated using a rotary evaporator. ? b* value indicates yellow while - a* value shows
green color and - b* value indicates blue color.
Mordanting Kubelka–Munk equation was used to measure the dye
absorption concentration on lyocell fabric surfaces in
The process of pre-mordanting was carried out in the terms of K/S values, as shown in Eq. (1) (Davulcu
shaker dyeing machine, and all fabric samples were et al. 2014).
treated with five chemicals (tin chloride, alum,
potassium dichromate, copper sulfate and ferrous K=S ¼ ð1 RÞ2 =2R ð1Þ
sulfate) with 6% on weight of fabric (OWF) at 90 °C where K, absorption; S, scattering coefficient; R,
temperature for 1 h. The pre-mordanting method was reflectance (McDonald 1997).
applied with material to liquor ratio 1:40. After
mordanting process, samples were washed with water
and dried at room temperature. Consequently, the
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4254 Cellulose (2018) 25:4251–4260
The antibacterial properties of pomegranate peel dyed The data in the figures are described by error bars
fabric were performed with agar diffusion test method. using standard deviation. The difference for samples
All samples (un-dyed, dyed with and without mor- data was obtained using ANOVA (one-way analysis).
danting) were selected for testing of antibacterial The data shown in figures are mentioned with p values
properties. Staphylococcus aureus (ATCCÒ 25923TM) such as (*) p \ 0.05, (**) for p \ 0.01 and (***) for
microorganisms were used in this test method. The p \ 0.001. However, the data differences were rec-
antimicrobial method, described in earlier studies, was ognized to be accurate if p (*) \ 0.05.
followed (Sanbhal et al. 2018b; Zhang et al. 2015).
First, 500 lL of bacterial suspensions (S. aureus
ATCCÒ 25923TM) was spread evenly onto the agar Results and discussion
plates then, lyocell dyed and white (control) samples
(1 9 1 cm) were placed onto surfaces of agar plates Lyocell fabric was used to dye with pomegranate peel
with a bacterial suspension (1 9 108 CFU/mL). extracted dye with and without mordanting agents.
Finally, after the incubation of samples at 37 °C for The dyeing process was carried out at temperature
18–24 h, the zone of inhibition diameter around the 90 °C for 1 h. It was observed that different colors
samples was measured with a digital vernier caliper. were obtained using different mordanting agents with
The zone of inhibition of incubated samples was same pomegranate natural dye. Antimicrobial proper-
calculated in four directions and reported as a mean ties of lyocell fabrics with pomegranate peel extracted
value. Equation (2) shows the formula which was used dye were studied. Thus, using the pre-mordanting
to calculate zone of inhibition of incubated samples method, the effects of different chemicals on color-
(Sanbhal et al. 2018b). fastness and color values were also examined.
L ¼ ðA DÞ=2 ð2Þ
Color efficiency and color values of dyed samples
where L, zone of inhibition; D, diameter of the dyed
and control sample before incubation; A, diameter of Figure 1 displays the lyocell fabrics dyed using
the tested samples with inhibition zone diameter. pomegranate peel with and without mordants. Thus,
To analyze the inhibition efficiency control and different mordanting agents displayed different colors
pomegranate peel dyed lyocell samples were after dyeing as well as the depth of shades changed
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Cellulose (2018) 25:4251–4260 4255
dramatically at same concentration of pomegranate efficiency (4.3) comparative to the copper sulfate
peels extracted dye. Moreover, Fig. 2 shows the color (CuSO4) (3.6) and Alum (KAl (SO4)212H2O) (2.7).
efficiency (K/S) values of dyed lyocell fabric using As shown in the Fig. 2 dyed lyocell fabrics
pomegranate extracted dye with and without chemi- demonstrated good color efficiency with chemicals
cals. The samples dyed with pomegranate peel but especially through the mordant stannous chloride.
using mordanting agents demonstrated better results Thus, color efficiency (K/S) of lyocell fabrics dyed
than without mordanting. Thus, K/S values of mor- with pomegranate peel indicated that different colors
danted dyed lyocell fabrics were found greater as were obtained with different mordanting agents.
compared to those dyed without mordants. However, However, in all conditions, the fabrics dyed with
among mordanting the chemical stannous chloride mordants showed greater color efficiency than without
(SnCl2) displayed higher K/S value (6.4) than all other mordanting dyed fabrics.
dyed samples. Potassium dichromate (K2Cr2O7) has Table 2 presents the outcomes of color efficiency
the lowest color efficiency (2.2) in all mordants. (L*, a*, b*, C*, h*) of dyed lyocell fabrics with and
Ferrous sulfate (FeSO4) has revealed better color without mordants. The color range of dyed lyocell
fabrics with pomegranate peel exhibited that mostly a
yellow (b*) color was observed in all shades. Treating
lyocell fabrics with different chemicals such as the
mordant stannous chloride shows highest color effi-
ciency (K/S = 6.4) of lyocell dyed fabrics than all
other dyed fabrics. However, the sample without
mordant shows lowest color efficiency (K/S = 1.2).
Moreover, there was no much difference in color
efficiency of fabrics dyed with pomegranate peel using
Alum (K/S = 2.7) and potassium (K/S = 2.2) as
mordanting agents. It can be observed that all samples
dyed with pomegranate peel shown higher K/S values
than samples dyed without mordants. Therefore,
mordanting process was necessary to increase the
color efficiency of lyocell dyed fabrics.
According to the L*a*b* values and chroma C*,
Fig. 2 K/S values of lyocell dyed fabrics with different
when assessing separately, it was confirmed that
mordants. In this figure, the statistical difference is shown as
p value (***), where p \ 0.001 (n = 3) stannous chloride was slightly redder showing 3.63
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red (a*) and 34.52 yellow (b*) with maximum chroma samples using ferrous sulfate (Fig. 3f) exhibited
(C*) 34.71 among all pomegranate peel dyed samples. second highest inhibition zone diameter of 1.5 mm
On the contrary, ferrous sulfate sample displays after stannous chloride (Fig. 3g) which demonstrated
reduced yellow (b*) values up to 11.90 and only greater average inhibition zone (1.60 mm) than all
2.07 redder (a*) with minimum chroma (C*) value of dyed samples. It has been observed from the Fig. 1 and
12.08. Moreover, samples dyed with copper sulfate Table 2 that K/S values of stannous chloride and
were turned to slight orange with 25.91 yellow (b*), ferrous sulfate were greater than all pomegranate peel
2.9 redder and second highest chroma (C*) value of dyed samples. Therefore, it can be summarized that
25.91 among all dyed samples. On the other hand, pomegranate peel dyed samples with higher K/S
pomegranate peel dyed samples using alum (KAl values also showed greater inhibition zone diameter.
(SO4)2.12H2O) were recorded more greener as com- Thus, as K/S values increase the antibacterial effi-
pared to all other dyed samples confirming 0.76 values ciency of pomegranate dyed samples also increased.
of (a*) redder, 23.70 yellower (b*) and chroma (C*)
value of 23.70. Moreover, fabrics dyed with pome- FTIR results
granate peel using potassium dichromate showed
slightly greener than non-mordanting dyed sample Figure 4 shows the structure of un-dyed lyocell fabric
with moderate chroma (C*) values of 20.27. and dyed lyocell fabric with pomegranate peel were
analyzed with FTIR (ATR). However, no any signif-
Antibacterial activity of lyocell dyed and un-dyed icant change in the bands was detected before and after
fabric dyeing. The bands at 3441 cm-1 and 3488 cm-1 can
be observed in all dyed fabrics. Such change was due
Antibacterial properties of dyed and un-dyed lyocell to the OH intermolecular hydrogen bonding. How-
fabrics are shown in Fig. 3. It can be observed that un- ever, a vibration band at 2892 cm-1 has confirmed the
dyed fabric sample (Fig. 3a) indicated slightly C–H bending. The peaks at 1645 cm-1 were observed
antibacterial activity against S. aureus ATCCÒ in all the samples ascribed water absorbance from the
25923TM). cellulose. All six tested samples have exhibited similar
However, pomegranate peel dyed fabrics has stretch peak bands at 1422, 1367 and 1315 cm-1
displayed improved antibacterial activity. The average which confirmed the CH2 symmetric bending, CH
inhibition zone diameter for the un-dyed lyocell fabric bending and CH2 wagging, respectively in Fig. 4.
was 0.2 mm. The lyocell samples dyed without The peak band at 1156 cm-1 shows asymmetric
mordant (Fig. 2b) demonstrated an average inhibition C–O–C stretching. While peak height at 1070 and
zone diameter of 1.4 mm. Moreover, lyocell samples 1028 cm-1 displayed the C–O group of lyocell
dyed with pomegranate peel (Fig. 2c) containing fabrics. Moreover, glucosidic bonds and vibration
potassium dichromate as mordant shown lowest bands at 895 cm-1 were also observed in all lyocell
inhibition zone diameter of 0.6 mm. Nevertheless, dyed and un-dyed fabrics. Thus, FTIR results in
pomegranate peel dyed lyocell fabrics using alum Fig. 4 revealed that the structure of lyocell fabric was
(Fig. 3d) and copper sulfate (Fig. 3e) as mordanting unchanged after dyeing with pomegranate peel. Dye-
agents displayed average inhibition zone diameter of ing method has not damaged the structural properties
1.2 and 1.3 mm, respectively. However, lyocell dyed of lyocell (lyocell) fibers. However, we found slight
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Cellulose (2018) 25:4251–4260 4257
Fig. 3 Antibacterial properties of lyocell dyed and un-dyed (KAl(SO4)212H2O), e copper sulfate (CuSO45H2O), f ferrous
samples a un-dyed, b dyed without mordant, c dyed with sulfate (FeSO47H2O), g stannous chloride (SnCl2)
mordants potassium dichromate (K2Cr2O7), d dyed with alum
vibration bands from 1645 to 1648 cm-1. The change Washing fastness
may be due to the more water absorbance from the
cellulose. These results are also consistent with the Washing fastness of dyed lyocell fabrics with different
literature (Carrillo et al. 2004) and recently published mordanting agents is shown in Table 3. However,
a paper of cotton dyed with pomegranate peel washing fastness properties of pomegranate peel dyed
(Davulcu et al. 2014). fabrics using stannous chloride as mordant agent
displayed highest washing fastness rating than all
other dyed fabrics with different mordants. Dyed
Colorfastness properties of lyocell dyed fabrics sample without mordants has also shown good wash-
with pomegranate peel ing fastness (4–5) like other mordants potassium
dichromate, alum, ferrous sulfate and copper sulfate. It
Table 3 shows color fastness to washing, light, can be concluded from all results of washing fastness
rubbing and perspiration of all lyocell dyed fabrics. that dyed with and without mordants revealed good to
excellent washing fastness results.
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Table 3 Colorfastness properties of dyed lyocell fabrics with different mordanting agents
Mordants Washing fastness Light fastness Rubbing fastness Perspiration fastness
ISO 150-C10 ISO 105-BO2 ISO 105-X12 ISO 105-E04
Dry Wet Acidic Alkali
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Cellulose (2018) 25:4251–4260 4259
and colorfastness of pomegranate peel extracted dye Al-Zoreky N (2009) Antimicrobial activity of pomegranate
for lyocell fabrics. (Punica granatum L.) fruit peels. Int J Food Microbiol
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ISO 105-X12 (2001) Textiles–tests for color fastness. Part X12:
fabric dyed with pomegranate peel demonstrated color fastness to rubbing: test 1 (France: 2001)
suitable antibacterial activity against S. aureus ISO 105-C10 (2006) Textiles–tests for color fastness. Part C10:
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could be useful potential for the preparation of ISO 105-B02 (2014) Textiles–tests for color fastness. Part B02:
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Acknowledgments The research was supported by the dyeing with natural dye extracted from pomegranate (Pu-
Fundamental Research Funds for the Central Universities (No. nica granatum) Peel. Univ J Environ Res Technol
17D310503) and National Natural Science Foundation of China 1:135–139
(No. 51403032). Lansky EP, Newman RA (2007) Punica granatum (pome-
granate) and its potential for prevention and treatment of
Compliance with ethical standards inflammation and cancer. J Ethnopharmacol 109:177–206
Lee Y-H, Hwang E-K, Kim H-D (2009) Colorimetric assay and
Conflict of interest The authors declare that they have no antibacterial activity of cotton, silk, and wool fabrics dyed
conflict of interest. with peony, pomegranate, clove, coptis chinenis and gall-
nut extracts. Materials 2:10–21
Mahmood MA, Al-Dhaher ZA, AL-Mizraqchi AS (2010)
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