Eco-friendly and protective natural dye from red prickly pear (Opuntia Lasiacantha Pfeiffer) plant

Abstract

New natural dye extracted from red prickly pear was used for dyeing wool with different types of mordents. The effect of mordant concentration on the color strength was discussed; the results obtained indicated that the color strength decreases with the increase of mordant concentration. The effect of the dye bath pH, salt concentration, dyeing temperature and dyeing time was also studied. The color strength and the dye uptake have exhibited high values. Good fastness properties of the dyed fabric were achieved.Antimicrobial activity of wool fabric dyed with this dye was tested according to diffusion agent. Test organisms as Escherichia coli, Bacillus subitilus, Pseudomons aeruginosa and Staphylococcus aureus were used and the results indicated that the samples exhibited a high inhibition zone.According to the available literature, this is the first report concerning a natural dye for fabric from fruits of red prickly pear plants.

Full text

ORIGINAL ARTICLE
Eco-friendly and protective natural dye from red
prickly pear (Opuntia Lasiacantha Pfeiffer) plant
N.F. Ali
a,
*
, R.S.R. El-Mohamedy
b
a
Dyeing and Printing Department, National Research Center, Dokki, Cairo, Egypt
b
Plant Pathology Department, National Research Center, Dokki, Cairo, Egypt
Received 22 September 2010; accepted 4 October 2010
Available online 20 October 2010
KEYWORDS
Red prickly pear;
Natural dye;
Dyeing wool;
Mordents;
Fastness properties
Abstract New natural dye extracted from red prickly pear was used for dyeing wool with different
types of mordents. The effect of mordant concentration on the color strength was discussed; the
results obtained indicated that the color strength decreases with the increase of mordant concentra-
tion. The effect of the dye bath pH, salt concentration, dyeing temperature and dyeing time was also
studied. The color strength and the dye uptake have exhibited high values. Good fastness properties
of the dyed fabric were achieved.
Antimicrobial activity of wool fabric dyed with this dye was tested according to diffusion agent-
ed. Test organisms as Escherichia coli, Bacillus subitilus, Pseudomons aeruginosa and Staphylococcus
aureus were used and the results indicated that the samples exhibited a high inhibition zone.
According to the available literature, this is the first report concerning a natural dye for fabric
from fruits of red prickly pear plants.
ª 2010 King Saud University. Production and hosting by Elsevier B.V. All rights reserved.
1. Introduction
Red prickly pear (Opuntia Lasiacantha Pfeiffer) is one of the
plants of cactacoae family. The plant grows in many parts of
the world such as Africa, Australia and the Mediterranean ba-
sin. In recent years according to field observations the area of
prickly pear cultivation was increased rapidly with reclamation
of new lands in the desert in Egypt. The fruits of the plant
(Fig. 1) are used for many foods and medical industries.
Prickly pear juice is used as a natural dye. Betalain pig-
ment was isolated from prickly pear (Fernandez-Lopez and
Almela, 2001; Forni et al., 1992), it is found also in red beets
(Beta vulgaris). The betalains are a group of nitrogen contain-
ing pigments that are yellow, orange, pink, red and purple in
color. Betalains have no toxic effects in the human body and
are seen as a natural and safe alternative to synthetic red col-
oring (Pigi et al., 2003; Ramadan and Morsel, 2003a,b). In
food industry, there is a growing tendency to replace synthetic
dyes by natural pigments as red prickly pear (Cai and Corke,
2000; Saenz, 2002). Betalains are cationized compounds with
*
Corresponding author. Tel.: +202 3370931, fax: +202 3370951.
E-mail address: aali_04@hotmail.com (N.F. Ali).
1319-6103 ª 2010 King Saud University. Production and hosting by
Elsevier B.V. All rights reserved.
Peer review under responsibility of King Saud University.
doi:10.1016/j.jscs.2010.10.001
Production and hosting by Elsevier
Journal of Saudi Chemical Society (2011) 15, 257–261
King Saud University
Journal of Saudi Chemical Society
www.ksu.edu.sa
www.sciencedirect.com

positive nitrogen in polyene system. 5-O –glucose betanidine
(1) are the pigments of the cactus pear fruit. The main fox of
interest, however, has recently been on betalain pigments as
antioxidants (Stintzing et al., 2001; Stintzing et al., 2003). Bet-
alains stability is affected by temperature, pH, oxygen, light,
and aqueous activity. The use of prickly pears as a source of
betalains may be interesting comparing with red beets since
the plants of the Opuntia genus need mineral requirements
from soil and water. This way may be a great alternative to
agricultural economy in arid and semiarid regions (Castellar
et al., 2003).
In the present paper betalain pigment extracted from red
prickly pear juice was used with different mordents as natural
dye for dyeing wool.
2. Experimental
2.1. Fruits of red prickly pear plant
The fruits of red prickly pear plant were collected from differ-
ent locations of Nobaria region (Beheria governorate at North
West of Delta, Egypt) .The juice of mature fruits was used as
natural source of dyes and anti fungal, anti bacterial agents
against some microorganisms in other studies.
2.2. Extraction
The peeled fruits of red prickly pear were homogenized with an
equal amount of water. The mixture was heated for 5 min at
80 C and quickly cooled on an ice bath until it reached a tem-
perature of 8–10 C then the extract was centrifuged for 20 min
(Butera et al., 2002).
2.3. Materials
Betalain pigment extracted from red prickly pear was used as a
natural dye; the chemical structure of this pigment is derived
from betalamic acid on the united components to this structure
(Fig. 2).
Scoured and bleached wool fabric with the following char-
acteristics was purchased from Misr for Spinning and Weaving
Company, Mahalla El-Kobra, Egypt; weight 205 g m
2
,72
ends per inch, 64 picks per inch. Before using, the fabric was
treated with a solution containing 5 g L
1
non-ionic detergent
(Hostapal CV, Clariant), at 50 C for 30 min.
Then, the fabric was thoroughly washed with water and air
dried at room temperature.
2.4. Mordanting
Pre and post mordanting were done by using different mor-
dents, namely, ferrous sulfate, copper sulfate, potassium
dichromate and tannic acid with concentrations varied be-
tween (20, 40, 60, 80, 100) g/kg at optimized extraction and
dyeing conditions (Bechtold et al., 2003; Bechtold et al., 2006).
2.5. Dyeing procedure
Wool samples were dyed using a dye bath containing different
amounts of sodium chloride (0–20 g L
1
) and the calculated
amount of the dye with liquor ratio 40:1, heating at different
duration (12–120) min and different temperatures (30–100 C).
The dyed samples were rinsed with cold water, washed in a
bath at liquor ratio 40:1 containing 3 g/L
1
non ionic deter-
gent (Hostapal CV, Clariant) at 50 C for 30 min, then rinsed
and finally dried at ambient temperature.
The pH values were recorded with Hanna pH meter and ad-
justed with dilute solutions of sodium carbonate.
2.6. Color strength
The reflectance of the soaped samples was measured on a
Perkin–Elmer Lambda 3B UV/Vis spectrophotometer. Rela-
tive color strengths (K/S values) were determined using the
Kubelka–Munk equation (Judd and Wysezchi, 1975).
K=S ¼
ð1  RÞ
2
2R

ð1  RÞ
2
2R
0
ð1Þ
where R = decimal fraction of the reflactance of dyed fabric,
R
0
= decimal fraction of the reflactance of undyed fabric,
K = absorption coeffictent, and S = scattering coefficient.
2.7. Fastness testing
The dyed samples were tested according to ISO standard meth-
ods. The specific tests were: ISO 105 X12(1987), color fastness
to rubbing; ISO 105-C02(1989), color fastness to washing; ISO
105-E04(1989), color fastness to perspiration; and ISO 105-
B02 (1988), color fastness to light (carbon arc)(Handbook
of Textite testing, 1988).
3. Results and discussion
The obtained results suggest that the colorant from red prickly
pear can be considered a potential source of natural food col-
oring (Fernandez-Lopez and Almela, 2001; Kanner et al.,
2001). In our study, betalain pigment extracted from red
prickly pear is used for dyeing wool; this dye is water soluble
and has to be fixed to make the color fast or permanent, using
fixatives or mordents, and it is stable in pH range of 4–7.
Figure 1 Red prickly pear fruit.
N
N
+
COOHHOOC
COO-
H
H
Figure 2 Betalain pigment structure.
258 N.F. Ali, R.S.R. El-Mohamedy

The stability of this dye was pH dependant and showed a
maximum at pH 5 as shown in Fig. 3.
3.1. Dyeing
Reduction in the color strength with excess concentration of
mordents (Figs. 3 and 4) was due to the aggregation of the ex-
tract molecules by the addition of excess metallic salts, causes a
reduction in the extract solubility, which leads to its precipita-
tion and difficulty of penetration during dyeing.
3.1.1. Effect of mordents (type & conc.)
The colors produced from using different types of mordents
are illustrated in Table 1.
3.1.2. Effect of pre and post mordenting
In the cases of pre and post mordenting, the K/S values in-
creases with an increase in the percentage of the mordant until
4% concentration is achieved as shown in Figs. 3 and 4,By
using a 4% solution of mordant, the results are even. After
that unevenness, it is observed that there are no differences
in the shade of the samples dyed with mordant solution and
those dyed without a mordant solution. It is clear that the
K/S values decrease as the concentration of the mordant in-
creases. It might be possible that the complex formed between
fabric and mordant is too strong. The affinity formed between
fabrics and mordant was strong .The affinity between the fab-
ric and mordant increased as we increased the concentration,
so that a stable complex was formed. Then when this mordent-
ed fabric was treated with dye extract, the dye was more rushed
towards the fabric and caused unevenness. From the Figs. 3
and 4) it is clear that maximum K/S is obtained for samples
dyed with a 4% mordant concentration and then after that
unevenness appears but the shade remains approximately the
same.
The reduction in the K/S with an excess concentration of
mordents is due to the aggregation of the extract molecules
by the addition of excess metallic salts, which causes a reduc-
tion in the extract solubility, and leads to its precipitation and
difficulty of penetration during dyeing.
Effect of pre and post mordenting was also investigated for
dyeing at optimum conditions. It is found that post-mordent-
ing gives maximum colour strength as compared to pre-mor-
denting. The colour strength values are given in Figs. 3 and
4. Low colour strength in pre-mordenting condition is due to
accumulation of the metal dye complex in the form of clusters,
which upon investigation in spectra flash spectrophotometer
show dull red and blue shades as shown in Table 2.
The above mordents used had the affinity for both the col-
oring matter and the fiber. The COOH groups present in the
extract structure might affect greatly its sensitivity to the addi-
tion of metallic salts, and the efficiency of metal complex
formation.
3.1.3. Effect of dye bath pH
Fig. 5 shows that the pH values of the dye bath have a consid-
erable effect on the dye ability of wool fabrics using the prickly
pear dye. The effect of the dye bath pH can be attributed to the
0
10
20
30
40
50
60
70
80
90
100
control
246 8
Post -mordanting conc.(%)
K/S (%)
1
2
3
4
Figure 4 The effect of the type of post mordant on the color
strength Fig. 2: The effect of the type of pre mordant on the color
difference values at different concentrations of mordants. 1-
ferrous sulphate, 2-potassium dichromate, 3-copper sulphate, 4-
tannic acid.
0
10
20
30
40
50
60
70
80
90
control 2 4 6 8
K/S (%)
Pre-mordanting conc.(%)
1
2
3
4
Figure 3 The effect of the type of pre mordant on the color
strength values at different concentrations of mordants. 1- Ferrous
sulphate, 2- Potassium dichromate, 3- Copper sulphate, 4- Tannic
acid.
Table 1 Colors produced from using different types of
mordents.
Type of mordents The produced color
Without mordant Yellow
Ferrous sulphate Yellowish brown
Copper sulphate Green
Potassium dichromate Olive green
Tannic acid Red
Table 2 Diameter of inhibition zone inhibition (mm) in the
diffusion agar test for the wool dyed with Perkily pear dye
against selected microbes.
Dye conc. (%) Diameter of inhibition zone (mm)
Tested microbes
E. coli B. sub. Ps. Au Sta. A.
0.5 7.54 22.3 8.5 7
1.0 12.6 21 13 8.7
2 13.5 27.9 18.32 15
0.0 6 8 4 0
Eco-friendly and protective natural dye from red prickly pear ( Opuntia Lasiacantha Pfeiffer) plant 259

correlation between dye structure and wool fabric. Since the
dye used is sparingly soluble in water, containing COOH
groups (Slawomir and Mizrahi, 2002; Castellar et al., 2003),
thus it would interact ionically with the protonated terminal
amino groups of wool fibers at acidic pH via ion exchange
reaction due to the acidic character of the COOH groups.
The anion of the dye has complex characters, and when it is
bound on the fiber, with ionic forces, this ionic attraction
would increase the dye ability of the fiber as clearly observed
in Fig. 5.
It was noticed from the figure that higher dye ability at pH
5, then the dye ability decreases due to decreasing the number
of protonated terminal amino groups of wool fibers, therefore
the ionic interaction decreases.
3.1.4. Effect of salt addition
Fig. 6 shows the effect of salt concentration on the color
strength obtained for the dyed fabrics. It is clearly indicated
that as the salt concentration increases the color strength de-
creases, it is also noticed that at zero concentration the value
of the color strength was maximum, i.e. dyeing without salt
addition is the best condition.
3.1.5. Effect of temperature
The effect of temperature on the dye ability of wool fabrics
with prickly pear dye was studied at different temperatures
(30–100 C). As shown in Fig. 7, it is clear that the color
strength increases with the increasing of dyeing temperature
and reaches to maximum value at 100 C.
3.1.6. Effect of dyeing time
As shown in Fig. 8, the color strength obtained increases as the
time increases up to 60 min, then it decreases, i.e, K/S displays
maximum in 60 min-dyeing time.
3.2. Antimicrobial activity
The antimicrobial activity of different concentrations of dye of
dyeing wool was studied. The data in Table 2 clearly show that
an increase in dye concentration leads to increased inhibition
zone of all tested microorganisms for dyed wool in comparison
to undyed wool. It may be concluded that a high inhibition
zone is recorded with 2% concentration. This indicates that
the prickly pear dye is highly effective antimicrobial against
all tested microorganisms. Bacillus subtilus and E. coli are
highly affected by the dye. Meanwhile, Staphyl A shows a
moderate effect.
3.3. Fastness properties
Fastness properties of the dyed fabrics are shown in Table 3.
The results indicate good fastness properties of the mordanted
dyed samples.
There was a relation between the dye mordant nature and
the dye removal under the influence of washing solution and
perspiration solution (acid and alkaline). This depends on
the groups capable to form hydrogen bonding and metal com-
plex. The higher the number of these groups the lower the
magnitude of the dye removal, thus mordanting with tannic
acid gave the highest washing fastness followed by potassium
dichromate, copper sulphate, ferrous sulphate and the unmor-
danting samples; the same results were found for perspiration
fastness.
K/S
pH
2
7
6
5
4
3
2
1
0
3
4
56 7
8910
Figure 5 Effect of dye bath pH on the color strength on wool
fabrics. Dyeing conditions: 2% shade, L.R 40:1, at 100 C, 40 min
for 1 h.
0
1
2
3
4
5
6
0 2.5 5 7.5 10 12.5
Salt conc.g/ l
K/ S
Figure 6 Effect of salt addition to the dye bath on the colour
strength of dyed wool. Dyeing conditions; 2% shade, L.R 40:1,
10 g L
1
sodium chloride, 1 h, at 100 C.
0
1
2
3
4
5
6
30 50 60 80 90 100
K/S
temperature
K/S
Figure 7 Effect of the dyeing temperature on the color strength
dyed wool fabrics. Dyeing conditions: 2% shade, L.R 40:1, pH 5,
1 h. 0 g salt conc.
0
1
2
3
4
5
6
30 40 40 60 80 100 120
Time(min.)
K /S
Figure 8 Effect of dyeing time on the color strength of dyed
wool fabrics. Dyeing conditions: 2% shade, L.R 40:1, pH 5 at
100 C, 0 g salt conc.
260 N.F. Ali, R.S.R. El-Mohamedy

Rubbing causes the removal of adhered molecules which
are most probably present as deposited layers on the fiber sur-
face, while those forming intermolecular hydrogen bonding or
being chemically combined with the fiber or forming metal
complexation are not removed by rubbing, thus samples mord-
anted by potassium dichromate, tannic acid, ferrous sulphate
and copper sulphate exhibited higher values of rubbing fast-
ness than unmordanted samples.
The light fastness of colorants tends to fall when their par-
ticle size decreases, provided that no interfering factors oper-
ate. The effect is clearly due to the greater specific surface of
colorants exposed to light; the increase of light fastness may
be a result of the decreasing surface activity of the dye mole-
cules and the increased dye–fiber bond strength, thus the light
fastness of the dyed samples showed very good (7–8, 8) fast-
ness with samples mordanted with potassium dichromate
and tannic acid and good fastness (7, 7) with samples mordant-
ed by copper sulphate and ferrous sulphate comparing with
unmordanted samples.
4. Conclusion
New red pigment was extracted from prickly pear juice and
used with different mordants as natural dye for dyeing wool
with good fastness properties and high dye uptake.
Antimicrobial activity of wool fabric dyed with this dye was
tested according to diffusion agented. Test organisms asE. coli,
B. subtilus Pseudomons aeruginosa and Staphylococcus aureus
were used and the results indicated that the samples exhibited
a high inhibition zone. Our study shows that natural red
prickly pear dye under investigation can provide bright hues
and color fastness properties. They can serve as a noteworthy
source of raw material in the future. Chemical modification of
natural compounds such as the dye in question could be an
interesting field of study as it could appreciably facilitate the
synthesis of dye molecule.
References
Bechtold, T., Turcanu, A., Ganglberger, E., Gessler, S., 2003. Natural
dye in modern textile dye houses- how to combine experiences of
two centuries to meet the demands of future? J.Clean. Prod. 11,
499–509.
Bechtold, T., Mahmud-Ali, A., Mussak, R., 2006. Natural dyes for
textile. A comparison of methods to assess the quality of golden rod
plant material. Dyes and Pigment 70, 1–7.
Butera, D., Tesoriere, L., Di Gaudio, F., Bongiorno, A., Allegra, M.,
Pintaudi, A.M., Kohen, R., Livrea, M.A., 2002. Antioxidant
activities of Sicilian Prickly Pear (Opuntia ficus indica) fruits
extracts and reducing properties of betalains: betanin and indica-
xanthin. J. Agric. Food Chem. 50, 6895–6901.
Cai, Y.Z., Corke, H., 2000. Production and properties of spary-dried
Amaranthus betacianin pigments. J. Food Sci. 56 (6), 1248–1252.
Castellar, R., Obon, J.M., Alacid, M., Fernadez-Lopez, J.A., 2003.
Color properties and stability of betacyanins from Opuntia fruits.
J. Agric. Food Chem. 51, 2772–2776.
Fernandez-Lopez, J.A., Almela, L., 2001. Application of high perfor-
mance liquid chromatography to the characterization of the
betalain pigments in prickly pear fruits. J. Chromatogr. 913, 415–
420.
Forni, E., Polesello, A., Montefiori, D., Maestrelli, A., 1992. A High
performance liquid chromatographic analysis of the pigments of
blood red prickly pear (Opuntia ficus indica). J. chromatogr. 593,
177–183.
Judd, D.B., Wysezchi, G., 1975. Color in Business, science and
Industry 3rd ed., John wiley & sons; New York. Handbook of
Textite testing, Part 4, 1st revision, Bureau of Indian standards,
New Delhi., 1988. pp. 115–119, 141–142.
Kanner, J., Harel, S., Granit, R., 2001. Betalains-a new class of dietary
cationized antioxidants. Agric. Food Chem. 49, 5178–5185.
Pigi, A., Del Caro, A., Pinna, I., Agabbio, M., 2003. Changes in
ascorbic acid, polyphenol content and antioxident activity in
minimally processed cactus pear fruits. Lebensmittel-Wissenschaft
under Technologie 36, 257–262.
Ramadan, M.F., Morsel, J.T., 2003a. Recovered lipids from prickly
pear (Opuntia ficus-indica) peel: a good source of polyunsaturated
fatty acids, natural antioxident vitamins and sterols. Food Chem.
83, 447–486.
Ramadan, M.F., Morsel, J.T., 2003b. Oil cactus (opuntia ficus-indica
L). Food Chem. 82, 339–345.
Saenz, C., 2002. Processing technologies: an alternative for cactus pear
(Opuntia spp.) fruits and cladodes. J. Arid Environ. 46, 209–225.
Slawomir, W., Mizrahi, Y., 2002. Fruit flesh betacyanin pigments in
hylocerus cacti. J. Agric. Food Chem. 50, 6086–6089.
Stintzing, F.C., Schieber, A., Carle, R., 2001. Phytochemical and
nutritional significance of cactus pear. Food Res. Technol. Int. 12,
6–407.
Stintzing, F.C., Schieber, A., Carle, R., 2003. Evaluation of color
properties and quality parameters of cactus juices. Eur. Food Res.
Technol. 216, 303–311.
Table 3 Fastness properties of dyed wool fabrics.
Types of mordents Washing Rubbing Perspiration Light fastness
ab
ACWRdRwACWACW
Without 3 3–4 3–4 3–4 3 3–4 3 3–4 3–4 3 4 6
Ferrous sulphate 4 4 4 4–5 4–5 4 4 4 4 4 4 7
Potassium dichromate 4–5 4–5 4–5 5 5 5 4–5 5 4 4–5 5 7–8
Copper sulphate 4–5 4–5 4–5 4 4 4–5 4–5 4–5 4 4–5 4 7
Tannic acid 5 5 5 4-5 4-5 5 4–5 5 5 5 5 8
A = change in colour, C = staining on cotton, W = staining on wool, Rd = dry rubbing, Rw = wet rubbing, a = acidic, b = alkaline.
Eco-friendly and protective natural dye from red prickly pear ( Opuntia Lasiacantha Pfeiffer) plant 261