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Chandrasekar S. et al. / International Journal of Biopharmaceutics. 2013; 4(3): 219-224.

e- ISSN 0976 - 1047


Print ISSN 2229 - 7499

International Journal of Biopharmaceutics


Journal homepage: www.ijbonline.com

IJB

HERBAL-CHITOSAN NANOCOMPOSITES FOR DURABLE


ANTIBACTERIAL FINISHING ON COTTON MATERIALS
1

Chandrasekar S*, 1Vijayakumar S, 2Rajendran R, 3Rajesh R, 4Elayarajah B


1

Department of Botany and Microbiology, A.V.V.M. Sri Pushpam College, Tanjore, Tamil Nadu, India.
2
PG and Research Department of Microbiology, PSG College of Arts and Science, Coimbatore, India.
3
Chief Scientist, R&d Bio, The Biosolution Company, Coimbatore, India.
4
School of Biological Sciences, CMS College of Science and Commerce, Coimbatore, India.

ABSTRACT
To enhance the efficiency of biological, chemical and physical properties of cotton fabrics by finishing with
chitosan and herbal extract nanocomposites. Senna auriculata and Achyranthes aspera extracts mixed with chitosan solution
was bulk finished directly on 40s cotton fabrics. With an objective to increase efficiency of the functional properties,
chitosan and herbal extract nanocomposites were finished on to another set of fabrics (nanocomposite finishing). Various
functional properties were analyzed and compared between both the sets of fabrics Antibacterial activity was carried out for
both before and after washed samples using standard EN ISO 20645 method and a standard AATCC - 147 test method
respectively. Physical properties like tensile strength, abrasion resistance and air-permeability were also analyzed.
Antibacterial activity of nanocomposite finished fabrics showed more inhibitory zones of 30.9 mm for E. coli and 28.9 mm
for S. aureus when compared to bulk finished fabrics which had a zone size of 24.9 mm for E. coli and 23.9 mm for S.
aureus. Similarly Nanocomposite finished fabrics showed good durable properties and physical properties than bulk
finished fabrics. The study concludes that, nanocomposites finish could provide better functional properties to the fabric
than the bulk finished material. The nanosized particles in the composites were considered significant for its functional
applications in hospital based fabrics to prevent the transmission of nosocomial infections.
Key words: chitosan, herbal extract, cotton, nanocomposite.
INTRODUCTION
Medical industry is challenged by the presence
of microorganisms and the negative effects they cause.
According to Williams et al., (2005) dramatic effects like
deterioration, defacement and odours which occur from
the microbial contamination of surfaces as varied as
carpeting and medical non-woven fabrics. Purwar and
Joshi, (2004) explained that these surfaces can also act as
a microbial harbour, as most offer ideal environments
Corresponding Author
Chandrasekar S
E-mail: sekar_biotech@yahoo.com

for the proliferation of microorganisms that are harmful


to buildings, textiles and humans. The ability to make
surfaces resistant to microbial contamination has
advantages in many applications and market segments.
Krueger, (2003) also confirmed that this is especially true
in medical markets where many products have
contributed a degree of aseptic sophistication beyond that
required of consumer products.
As consumers have become more aware of
hygiene and potentially harmful effects of microbes, the
demand for antimicrobial finished clothing is increasing
(Thilagavathi et al., 2007). In the development of fabrics,
functional aspects such as anti-bacterial and UV
protection are playing an increased important role

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Chandrasekar S. et al. / International Journal of Biopharmaceutics. 2013; 4(3): 219-224.

(Kwong, 2006). Though chemicals and heavy metal


finished fabrics provide good antimicrobial activity, due
to factors like toxicity, and non-biodegradability, they
cannot be used for medical applications. Hence, natural
polymers like chitosan and herbal extract finished fabrics
were considered significant for medical applications.
Chitosan derived from acetylation of chitin, the marine
polymer was a best alternative for heavy metals in
finishing the medical fabrics. Chitosan is a natural, nontoxic, microbial resistant biodegradable polymer. Its
derivatives as antimicrobial agents have received more
attention to finish antimicrobial textiles. Similar effects
from the extracts of medicinal plants like Senna
auriculata and Achyranthes aspera were also considered
significant for the functional finishing of textile materials
for antibacterial, antifungal and anti odor properties.
Even though reactive exhaust method and
microencapsulation method have been used extensively
in textile industries for functional finishing of fabrics, a
novel technique called nanoencapsulation is rapidly
emerging and widely used in pharmaceutical, chemical,
cosmetics and food processing industries (Wang,
2005).More recent years the method was also expanded
to textile finishing industries due to its significant binding
properties on cellulosic substrates. Nanoencapsulated
drugs after finishing onto the textile materials provides a
slow and controlled release of the active antimicrobial
ingredient to achieve the desired delay until the right
stimulus is obtained (Nataporn Sowasod, 2006).
Nanocomposites are formed by the combination of two or
more materials that have quite different properties. These
different materials work together to give the unique
properties of the composite which is the materials
individual properties (Rajendran, 2012).
Considering the significant characteristics of
this technique, in our present research, chitosan and
herbal extract nanoparticles were prepared and were
functionally finished on the cotton fabrics. To find out
the efficiency of nanocomposite finished cotton fabrics,
the parameters like antibacterial activity, wash durability
and physical properties was compared with chitosan and
herbal extracts (bulk) finished cotton fabrics.
MATERIALS AND METHODS
The entire research work was carried out from
February 2012 to June 2013.
Materials used in the study
Fabric material selected for the study was plain
weave 40s medical grade cotton with 60 ends per inch
(EPI) and 56 picks per inch (PPI).
Medicinal plants and chitosan
Two medicinal plants, Senna auriculata,
Achyranthes aspera and a natural polymer chitosan were
collected from Department of Plant Science, Tamil Nadu

Agricultural University, Coimbatore, India. Leaves of the


plants were used in the study.
Test bacterial cultures
The test cultures, Escherichia coli and
Staphylococcus aureus used in the study were the
significant pathogens isolated from the wound dressing
fabric materials of a diabetic foot.
Preparation of antibacterial agents
Methanol extracts of medicinal plants (Thilagavathi
and Kannaian, 2008)
Fresh leaves of Senna auriculata and
Achyranthes aspera was shadow dried at 37C. Drying
was done to reduce the moisture content of leaves to less
than 20%. Dried leaves were grounded to make fine
powder for the extraction of desired materials. Fine
powdered material was extracted to obtain the active
substances with suitable solvent (methanol). 10 grams of
powdered leaves of Senna auriculata were extracted in
100ml of 80% methanol for 18 hours under shaking
condition. For every 6 hours the solution was sonicated
for 20 minutes to obtain the exact antibacterial substances
of the medicinal plants. Similar procedure was carried
out for 10 grams of powdered leaves of Achyranthes
aspera
Preparation of Chitosan solution (Rajendran et al.,
2012)
Chitosan (1%) solution was prepared by mixing
with acetic acid (1%) and stirred in a magnetic stirrer at
60C till a fine homogenous suspension was formed. The
polymer solution was kept overnight at stand still
condition to remove air bubbles formed during stirring.
Preparation of antibacterial nanoparticles
Herbal extract nanoparticles (Sumithra and Vasugi
Raaja, 2012)
Herbal extract nanoparticles were prepared by
coacervation
process
by
cross-linking
with
glutaraldehyde for both herbs separately. In this method,
the herbal extract was incubated with bovine serum
albumin (wall material 2% w/v) for one hour at room
temperature. Using 1M HCl pH was adjusted to 5.5.
Ethanol was added to the solution in the ratio of 2:1 (v/v)
at the rate of 1ml/min. Coacervate thus formed was
hardened with 25% glutaraldehyde for 2 hours to allow
cross-linking of protein. Organic solvents were removed
by rotary vacuum evaporator and resultant nanocapsules
were purified by centrifugation at 4 C at 10,000 rpm.
Pellets were suspended in 0.1M PBS (pH 7.4) and
lyophilized with mannitol (2% w/v).
Chitosan nanoparticles (Rajendran et al., 2012)
Chitosan nanoparticles were prepared
emulsion method. Briefly, 100ml of 1.5%

by
of

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tripolyphosphate solution was added into chitosan


solution (100ml of 2mg/ml in 1% diluted acetic acid) at a
rate of 10ml/min under constant stirring condition till a
milky emulsion was obtained (pH-5.0). The emulsion
was frozen at -4C followed by thawing in the
atmosphere to get solid nanoparticles. The emulsion was
centrifuged at 10,000 X for 30 min. Finally, the deposited
nanoparticles were washed, vacuum dried at 60C for 18
hours and stored at 4C.
Bulk and nanocomposite finishing of cotton fabrics
Two sets of fabric samples were used in this
study. In the first set of samples the prepared antibacterial
agents were directly finished (bulk finishing) with herbal
extracts of Senna auriculata and Achyranthes aspera and
chitosan). In the second set of fabric samples, similar
herbal nanoparticles and chitosan nanoparticles
(nanocomposite finishing) were finished. All the samples
were padded with 8% citric acid in a padding mangle at a
pressure of 3 psi with 100% wet pickup followed by
drying and curing at 160C for 5 min.
Comparative analysis of bulk and nanocomposite
finished cotton fabrics
Fabrics finished with antibacterial agents and
with antibacterial nanoparticles were compared for
different biological and physical properties.
Antibacterial assessment of the finished fabric (EN
ISO 20645 test method)
The antibacterial activity of two sets of finished
fabric (bulk and nanocomposite) was tested according to
EN ISO 20645 against the test bacterial cultures,
Escherichia coli and Staphylococcus aureus. The
finished cotton fabric with the diameter of 20 1 mm
was placed on the surface of Nutrient agar medium which
was swabbed with the bacterial cultures. The plates were
incubated at 37 C for 24 hours to measure the zone of
inhibition in millimeters formed around the fabric.
Wash durability of finished fabric (AATCC 124 test
method)
Bulk and nanocomposite finished cotton fabrics
were analyzed for their wash durability by subjecting the
sample to repeated washing and antibacterial testing
using the standard AATCC-124 and AATCC 147 test
methods (Parallel streak method). All the samples were
washed and its antibacterial activity was analyzed after
1st, 5th and 10th wash.
Physical properties of finished cotton fabrics
Difference in the physical properties of two sets
of finished fabrics was analyzed with untreated control
cotton samples. Four significant parameters which were
considered for comfort properties of cotton fabric were
selected for the study. Tensile strength is the measure of

the resistance of the fabric tensile load or stress in either


warp or weft direction. Abrasion test was determined the
ability of a fabric to withstand damage by friction. Air
permeability of a fabric is the volume of air measured in
cubic cm passed per second through 1 sq. cm for the
fabric at a pressure of one cm. head of water. Also the
difference in the weight of the finished fabrics was
measured to determine the presence of antibacterial
agents. Tensile strength, abrasion resistance and airpermeability were analyzed using the standards, ASTM
D 5035-2006, AATCC 119-2004 and ASTM D 737-1996
respectively.
RESULTS AND DISCUSSION
In the present study, bulk finished and
nanocomposite finished cotton fabrics were analyzed to
determine their efficiency of biological and physical
properties. Antibacterial activity and the durable
properties of the nanocomposite finished cotton fabrics
were analyzed along with physical properties like air
permeability and abrasion resistance to determine the
regular use of the finished fabric for hospital workers and
patients.
Antibacterial assessment of the finished fabric by EN
ISO 20645
Two sets of finished fabric were assessed for
their antibacterial activity by EN ISO 20645 against test
bacterial cultures. The zone of inhibition for the first set
of bulk finished fabric was 24.9 mm and 23.9 mm for E.
coli and S. aureus respectively (Table-1). Second set of
fabric treated with nanocomposites showed more
inhibitory zones than the first set of finished fabric
against same test bacterial cultures.
Nanocomposite finished fabric inhibited the organisms
with the zones of 30.9 mm for E. coli and 28.9 mm for S.
aureus (Figure-1). The measured zone of inhibition thus
indicated that nanocomposites not only prevented the
growth under the fabric also it constantly leached out
from the material by restricting the growth of organisms
to a greater extent than the first set of finished fabric.
Wash durability of finished fabrics (AATCC 124
test method)
Difference in the durable properties between
two sets of finished fabric was analyzed by repeated
industrial washings. Durability was tested based on their
antibacterial activity using standard Parallel streak
method (AATCC 147 test method). First set of bulk
finished fabric showed inhibitory zones of 26.3 mm, 25.9
mm and 25.6 mm for E. coli and 27.6 mm, 26.3 mm and
25.6 mm for S. aureus after 1st, 5th and 10th wash
respectively (Table-2). Whereas the second set of
samples (nanocomposite finished) provided more
inhibitory zones than the first set of finished fabric. After
10th wash, the inhibitory zone of 26.3 mm and 26.9 mm

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was reported for E. coli and S. aureus (Figure-2) whereas


comparatively less inhibitory zone was observed for the
bulk finished fabric against the test cultures. This showed
that the nanocomposite fabric was able to retain the
antibacterial activity even after 10 industrial washes,
thereby providing long term durability of the
nanocomposite finished fabric.
Nano-sized particles of chitosan and herbal
extracts played a vital role in providing the durability in
finished fabrics. Nanosized particles due to their low
concentration also considered significant in reducing the
colour in finished fabrics. The colour of plant extracts
was a widely-met problem in the applications of textile
because treated cotton often change to green colour since
higher concentration of crude extracts were used for
finishing the fabrics. In the present study nanocomposites
containing low concentration of antibacterial agents were
finished which provided more antibacterial activity with
greater durable properties. Durability of fabric treated
with nanoparticles was mainly due to their size of nature
in which they are present in the cotton fabric. The
nanosized particles embedded easily within the cellulose
moieties of cotton, so that it remains constant and
released at low concentrations which ultimately required
for inhibiting the growth of organisms
Physical properties of finished cotton fabrics
The physical properties of the nanocomposite
finished fabric and bulk finished fabric was compared
with untreated control cotton fabric in Table-3. The
tensile strength of nanocomposite finished cotton fabrics
was found to be similar to untreated control cotton
fabrics. Due to nanosized particles the nanocomposite
finished fabrics does not vary with the tensile property of
untreated control cotton fabrics. Whereas tensile strength
of bulk finished fabric showed slightly higher tensile
strength to the tune of 3.65 % as compared to that of
untreated cotton fabrics. This was mainly due to the

larger size and concentration of the particles that was


finished in the fabrics. No change in the abrasion
resistance was detected for both the finished fabrics when
compared to the untreated cotton after 5 hours at 18000
rpm. Similarly, no significant difference in the weight
between the nanocomposite finished fabric and untreated
control cotton fabric was detected. After finishing with
either bulk particles or nanocomposites, addition of
antibacterial agents on each fabric samples was
calculated. The weight of the samples was measured
before and after finishing individually with bulk particles
and nanocomposites. Bulk finished samples showed more
fabric weight than the nanocomposite finished fabric
samples. In this regard, the bulk finished samples showed
3.08% and 2.27% more weight than unfinished and
nanocomposite finished samples respectively. Whereas,
nanocomposite finished samples showed only 0.82%
more weight than the unfinished samples.
The results indicated that nanocomposite
finished fabric may strongly influence the comfort
properties of the wearer. Air-permeability which
ultimately tested to decide the comfort properties showed
interesting phenomenon of differences between bulk and
nanocomposite finishes. Bulk finished fabrics showed
relatively low air-permeability than the nanocomposite
finished fabrics. Air-permeability of bulk finished fabric
was 102cm3/cm2/sec which was 6.27% less than that of
untreated control cotton (95.6cm3/cm2/sec). Whereas the
nanocomposite finished fabric was measured as
96.6cm3/cm2/sec which was only 1.03 % less than the
untreated control samples, ensuring more airpermeability and also influencing the comfort property of
the fabric. This may be due to the particle size which was
considered to be in nano size; that may not block the
pores of fabrics. But the pores in bulk finished fabric may
get blocked due to the size of chitosan and herbal
particles, which in turn leads to low-permeability of air
thus decreasing the comfort properties of the fabric.

Fig 1. Antibacterial assessment of the nanocomposite


finished fabric

Fig 2. Wash durability of nanocomposite fabric

Assessment was made by EN ISO 20645 against two test


bacterial cultures E. coli and S. aureus

Durable properties were determined after antibacterial


assessment against E. coli and S. aureus.
Assessment was made using AATCC 147 parallel streak
method 5th wash fabric was presented in the figure

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Chandrasekar S. et al. / International Journal of Biopharmaceutics. 2013; 4(3): 219-224.

Table 1. Antibacterial assessment of the finished fabric by EN ISO 20645


Zone of inhibition (mm)
Test Culture
Escherichia coli#
Staphylococcus aureus#
Unfinished fabric
0
0
Chitosan finished
14.6
13.3
Herbal finished fabric
10.9
10.3
Chitosan+herbal (bulk) finished fabric*
24.9
23.9
Nanocomposite finished fabric*
30.9
28.9
* Values in mm was measured including the diameter size of the fabric (20 mm)
# Mean values were tabulated after performing three times for each test culture
Table 2. Wash durability of finished fabric by AATCC 124 test method
Zone of inhibition (mm) after washes (in numbers)
Escherichia coli#
Staphylococcus aureus#
Test Culture
st
th
th
st
1
5
10
1
5th
#
#
#
#
Unfinished fabric
25
25
25
25
25#
Chitosan finished fabric
26.3
25.9
25.6
26.6
26.0
Herbal finished fabric
26.6
26.3
25.9
26.9
26.3
Chitosan+herbal finished fabric*
26.3
25.9
25.6
27.6
26.3
Nanocomposite finished fabric*
27.6
26.6
26.3
28.3
26.9
* Values in mm was measured including the diameter size of the fabric (25 mm)
# No inhibitory zone was observed (value given is the actual diameter of the fabric)

10th
25#
25.3
25.3
25.6
26.9

Table 3. Physical properties of finished cotton fabrics


Physical properties

Bulk finished fabric

Tensile strength

35.6 kgf
No breakdown of the
specimen up to 18000 rpm
for 5 hours

Resistance to abrasion

Nano-composite finished
fabric
34.6 kgf
No breakdown of the
specimen up to 18000 rpm
for 5 hours

Fabric weight
74.6 gm / m2
72.9 gm / m2
Grams/Sq/Metre (GSM)
Air permeability
102 cm3/cm2/sec
96.6 cm3/cm2/sec
All the tests were tested in triplicates, Mean values were tabulated
CONCLUSION
In the present study, the advantages of
functionally finished nanoparticles on the medical cotton
were well determined based on the biological, chemical
and physical properties. The nano size of chitosan and
herbal extracts increases the durability and antibacterial
activity of finished fabric to a greater extend. Also, no
change in physical properties of nanoparticle finished
cotton could also influence its wide applications in the
hospitals for the workers and patients in providing
suitable comfort properties. As future perspective, the
biocompatible nature of herbal finished fabrics shall be
tested using any standard animal cell lines or Hens Egg
test-Chorio allantoic membrane (HET-CAM) test inorder

Untreated control cotton


34.3 kgf
No breakdown of the
specimen up to 18000 rpm
for 5 hours
72.3 gm / m2
95.6 cm3/cm2/sec

to determine the regular usage of diseased patients in


hospitals without any hypersensitivity reactions.
ACKNOWLEDGEMENTS
We thank, Department of Botany and
Microbiology, A.V.V.M. Sri Pushpam College, Poondi,
India for the preparation of Herbal extraction and
chitosan polymer solution. RndBio, Biosolution
Company at Coimbatore for the preparation of chitosan
and herbal extract nanocomposites Department of
Microbiology, PSG College of Arts and Science,
Coimbatore, India for finishing the fabrics with
antibacterial agents using padding mangle.

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