Thermal and Rheological Properties of the Mucilage From the Fruit of Cordia lutea

Thermal and Rheological Properties

of the Mucilage From the Fruit of
Cordia lutea
Omar P. Troncoso, Bruno Zamora and Fernando G. Torres*
Department of Mechanical Engineering, Pontificia Universidad Catolica del Peru, Lima
32 - Peru

Received: 20 February 2017, Accepted: 8 May 2017

Summary
In recent years, natural gums and mucilages have been shown to be useful in
the food and pharmacological industries. In this study, the mucilage of the fruit of
Cordia lueta has been extracted and characterised in order to explore its potential
applications. Thermogravimetric tests were used to measure the water content of
this natural mucilage. Differential scanning calorimetry allowed assessing thermal
transitions and thermal degradation of the samples. Steady flow rheometry was
used to measure the viscosity of the samples as a function of the shear rate.
Dynamic oscillatory rheometry was used to study the variation of the storage and
loss modulus of the mucilage as function of the oscillatory frequency and stress.
The results showed that this mucilage is a polysaccharide network that behaves
as a pseudoplastic fluid. Its storage modulus is not completely independent from
the oscillation frequency. In addition, the stress sweeps showed that C. lutea
mucilage has a reversible stress softening behaviour. The findings reported in the
present work suggest that this mucilage can be used as a rheology modifier for
commercial foods and biomedical materials.

Keywords: Mucilage; Cordia lutea; Rheology

INTRODUCTION
Fruit mucilages are polysaccharides formed by large molecules of sugars
and uronic acids joined together by glycosidic links [1]. Plant mucilages
can be extracted from a variety of parts, including rhizomes, roots and seed
endosperms [2]. Some mucilages are water-soluble and form viscous solutions;

*Corresponding author: fgtorres@pucp.pe

Smithers Information Ltd, 2017

Polymers from Renewable Resources, Vol. 8, No. 3, 2017 79

Omar P. Troncoso, Bruno Zamora and Fernando G. Torres

other mucilages are not-water soluble but swell and absorb considerable
quantities of water [3]. Mucilages are used in the medical and pharmaceutical
industry [4-6], food industry [7], agriculture [8], textile [9], paper [9] and cosmetics
industry [10]. Some advantages of these natural plant-based materials are
their biodegradability, biocompatibility, non-toxicity and low cost [11].
Cordia is a genus of trees or shrubs in the borage family Boraginaceae.
About 300 species have been identified worldwide [12]. Previous studies
report the characterization of mucilages extracted from different Cordia
species. Cordia myxa have fruits that contain a gum composed of an anionic
polysaccharide which is covalently bound with proteins [13]. The polysaccharide
is an arabinoglucan with the backbone of (1/6)-linked D-glucopyranosyl and
(1/2)-linked L-arabinofuranosyl residues [14]. The mucilage from Cordia myxa,
has been used to produce flexible, transparent films with excellent oxygen
barrier properties [15]. It has been reported that a gum extracted from C. Myxa
possesses excellent emulsifying properties and can be used as a coating material
on nuts to retard oxidative rancidity [16-19]. The gum extracted from Cordia
obliqua has been reported to be an excellent emulsifier and tablet binder [19].
In addition, this gum has been reported to be useful as coating to increase the
shelf-life and improve the stability of food containing a high lipid proportion [19].
The mucilage of Cordia abbysinica has been used as glue by rural school
children in southern Africa because of its excellent adhesive properties [19].
Cordia lutea is a flowering indigenous plant of South America. Its flowers
have been widely used in traditional medicine for the treatment of hepatic
disorders and scurvy (Vitamin C deficiency) [20]. The fruit of C. lutea is a
drupe about 20 mm in diameter with a mucilaginous flesh that is tacky and
highly viscous (Figure 1). As far as the authors are concerned, there is a lack

Figure 1. (a) External view of a C. lutea fruit, (b) Cross-sectional view showing the
mucilaginous flesh of a C. lutea fruit

80 Polymers from Renewable Resources, Vol. 8, No. 3, 2017

 Thermal and Rheological Properties of the Mucilage From the Fruit of Cordia lutea

of information regarding the structure and properties of C. lutea that would

allow effectively exploit its mucilage. The aim of this paper is to assess the
thermal and rheological properties of the mucilage extracted from the fruit
of C. lutea in order to explore its potential use in food, pharmaceutical and
other technical applications.

MATERIALS AND METHODS

Mucilage Extraction
Mucilage was expressed from the fruits by tincture press. Fresh and raw fruits
of C. lutea were collected in June 2016 and transported to the laboratory and
stored at 4C. The samples were weighed every day to assess any variation.
Variations in sample weight decreased after five days. Thermal and rheological
tests were performed after 5 days in order to minimize water desorption
during the tests.

Characterization Techniques

Thermal Analysis
Differential scanning calorimetry tests were performed in a DSC-4000 (Perkin
Elmer, USA) calorimeter. Samples of 9 mg in weight were first heated at
110C to remove all the evaporable compounds and then cooled at 30C for
5 minutes. Dry samples were heated from 30C to 400C with a heating rate
of 3C/min under nitrogen gas passing at a flow rate of 20 mL/min. Large
volume stainless steel pans were used. 5 samples extracted from 5 different
C. lutea fruits were tested.
Thermogravimetric analysis was performed in a TGA-4000 (Perkin Elmer,
USA). Samples of 9 mg in weight were heated from 30C to 220C using a
heating rate of 10C/min. 5 samples extracted from 5 different C. lutea fruits
were tested.

Rheological Tests
Measurements were made using an AR-550 (TA Instruments, USA) rheometer,
equipped with a 20 mm parallel plate fixture. Sand paper was glued to the
lower and upper plates in order to limit possible slippage between plates
and sample. For the steady flow measurements, the samples were sheared

Polymers from Renewable Resources, Vol. 8, No. 3, 2017 81

Omar P. Troncoso, Bruno Zamora and Fernando G. Torres

from 0.01 to 200 1/s. The apparent viscosity was registered as a function of
the shear rate.
Oscillatory tests were performed to measure the storage modulus (G) and
the loss modulus (G) of the samples. Frequency and stress scans were
performed. In order to determine the frequency and stress range for the tests,
avoiding wall slippage, stress sweeps were performed at different frequency
and stress levels. The induced stress was monitored and oscillations with a
nonsinusoidal fashion were considered as indicative of slippage. Each type
of scan was performed at least five times. Frequency scans were carried out
at 25C with a constant stress of 0.5 Pa. Frequency varied from 0.05 Hz to
40 Hz. Two steps were used in each stress scan. In the first step, the stress
varied from 0.1 Pa to 100 Pa. Immediately after the first stress finished, the
second step started with a stress of 100 Pa until 0.1 Pa was reached. For
both steps, temperature and frequency were kept constant at 25C and 1Hz,
respectively. A minimum of 5 samples extracted from 5 different C. lutea fruits
were used per condition.

RESULTS AND DISCUSSION

Mucilages are formed by polysaccharides which contain large number of
hydroxyl and carboxyl functional groups in their structure [21]. The FTIR
spectrum of the mucilage of C. lutea extracted in this study is depicted in
Figure 2. The band at 1050 cm-1 can be associated with the stretching vibration
of C-O-C [1]. The broad band centred at 3270 cm-1 is attributed to hydrogen
bonded O-H stretched vibrations. The bands at 2929 cm-1 and at 1723 cm-1
are associated to C-H and C=O stretching vibrations, respectively. The band
at 1723 cm-1 in combination with the bands at 3270 cm-1and 1587 cm-1
could be accounted for carbonyl-bands of carboxylic acids [22]. Carboxylic
acids have been found in the fruit of Cordia latifolia [23]. This spectrum is in
agreement with the spectra of mucilage extracted from other fruits [24, 25].
The mucilage extracted from C. lutea has the appearance of a viscous gel
formed by a network of polysaccharides chains. Figure 3 shows a representative
thermogram of a C. lutea sample. A continuous weight loss is observed
up to ~160C associated to the loss of water (Table 1). This first stage of
decomposition resulted in ~80% of weight loss. A second decomposition
stage was found after water evaporation had taken place, and was probably
related to breakdown of the polysaccharide chains of the C. lutea mucilage
resulting in the formation of some reasonably high molecular mass volatiles.
Figure 4 shows a representative thermogram of a mucilage sample. No melting
peak was observed in the thermogram. This suggests that the polymer in

82 Polymers from Renewable Resources, Vol. 8, No. 3, 2017

 Thermal and Rheological Properties of the Mucilage From the Fruit of Cordia lutea

Figure 2. FTIR spectrum of the mucilage extracted from the fruit of C. lutea

Figure 3. Variation of weight as function of temperature of the mucilage of C. lutea

Polymers from Renewable Resources, Vol. 8, No. 3, 2017 83

Omar P. Troncoso, Bruno Zamora and Fernando G. Torres

the mucilage is mainly composed of amorphous polymers. An exothermic

peak is depicted at around 158C and can be associated with the thermal
degradation of the polysaccharides of the mucilage, which is in agreement
with the TGA results.

Figure 4. Variation of heat flow as function of temperature of the mucillage of C. lutea.

An exothermic peak is observed at 158C

Table 1. Results of the TGA tests performed on C. lutea mucilage

Parameter Value
First stage mass loss (%) 79.5 4.2
Second stage onset temperature (C) 162.7 3.7
Second stage mass loss (%) 14.7 2.6
Total mass loss (%, at 500C) 92.3 1.1

The rheological properties of C. lutea mucilage were also assessed in order

to explore its potential applications. Figure 5 shows a representative plot of
the apparent viscosity of C. lutea mucilage as a function of the applied shear
rates. The viscosity of the samples decreases as the shear rate increases,
showing a pseudoplastic behaviour. Shear thinning has been reported for
other polysaccharide-based networks such as xanthan gum, cellulose gum
and Gum arabic [26-28]. In these networks, shear thinning occurs due to a
change in the orientation of polymeric chains which become increasingly

84 Polymers from Renewable Resources, Vol. 8, No. 3, 2017

 Thermal and Rheological Properties of the Mucilage From the Fruit of Cordia lutea

aligned in the direction of the flow as the shear rate increases. Due to this
alignment the polymeric chains offer less resistance to flow, which leads to
a decrease in viscosity.

Figure 5. Variation of the apparent viscosity as function of the shear rate of the
mucillage of C. lutea

The rheological properties of polymeric liquids are dependent on the

instantaneous number density of molecular entanglements [29]. According
to Rafe et al. [30], shear thinning of polysaccharide networks, occurs when
the rate of disentanglement by shearing forces becomes greater than the
rate of formation of new entanglements. Frequency sweeps were performed
to assess the relaxation phenomena that take place during the shearing of
C. lutea mucilage. Figure 6 shows a representative frequency sweep. For an
oscillatory frequency between 0.4 and 2.5 Hz, the storage modulus is nearly
frequency independent and the loss factor (=G/G), which is a measure of the
relative contribution of viscous components to the mechanical properties of
the material, ranges 0.03-0.06. This suggests that the mechanical behaviour
of the mucilage is predominantly elastic in this frequency range (0.4-2.5 Hz).
In contrast, for small (0.05-0.4 Hz) and high (2.5-40 Hz) oscillatory frequencies,
the storage and loss moduli are frequency dependent with a loss factor that
ranges 0.1-0.6. At high frequencies, the storage modulus of the C. lutea
mucilage decreases with frequency, suggesting that the physical joints in
the polysaccharide network are being destroyed. A relatively large frequency
dependence of the moduli, together with a relatively high loss factor (> 0.1),
is a typical feature of a so-called weak gel [31-33].
Figure 7 depicts the dependence of G and G with the oscillatory stress. The
storage modulus starts decreasing at around 10 Pa while the loss modulus

Polymers from Renewable Resources, Vol. 8, No. 3, 2017 85

Omar P. Troncoso, Bruno Zamora and Fernando G. Torres

Figure 6. Variation of the storage modulus (G), loss modulus (G) and loss factor as
function of the oscillation frequency of the mucilage of C. lutea

Figure 7. Stress dependence of the storage modulus (G) and loss modulus (G) of a
representative sample of the mucilage of C. lutea. The first step (filled symbols) was
performed with an oscillatory stress increase from 5 to 80 Pa and the second step
corresponds to a decrease in applied stress from 80 to 5 Pa. The test confirms the
existence of a reversible stress softening behaviour

decreases at around 12 Pa. This behaviour is termed Stress Softening and it

is typical of physical gels [34-36]. It associated with permanent disruption of
physical crosslinks [36]. If this softening permanently affected the physical
crosslinks of the C. lutea mucilage, this would permanently change the
structure of the gel but the same sample was tested several times and the
curves obtained were always the same (Figure 7), depicting a reversible
stress softening behaviour.

86 Polymers from Renewable Resources, Vol. 8, No. 3, 2017

 Thermal and Rheological Properties of the Mucilage From the Fruit of Cordia lutea

The mucilage of C. lutea is water soluble and could be used in the food industry
to modify the rheology of foodstuffs. It has been reported that the mucilage
from C. abyssinica has potential applications as thickener, emulsion stabiliser
and binding agent in the food industry [37-38]. The rheological tests carried out
here showed that C. lutea mucilage shows shear thinning flow behaviour, which
would provide C. lutea-based fluids with desirable mixability, pumpability and
pourability. In addition, the amount of hydrogen bond forming groups (carboxyl
and hydroxyl groups) determined by the FTIR tests confirm good bioadhesive
property for the mucilage of C. lutea. This suggests that C. lutea mucilage could
be used in the development of new materials for biomedical applications, such
as bioadhesives, wound care biomaterials and drug delivery systems.

CONCLUSIONS
In this study the mucilage of C. lutea has been characterized using a materials
science approach. The thermal analysis showed that the water content of the
mucilage is around 90%. An exothermic peak due to thermal degradation
was observed at 158C. The variation of the apparent viscosity with the
shear rate showed that the C. lutea mucilage behaves as a pseudoplastic
fluid. In addition, the frequency sweeps showed that the storage modulus is
frequency independent only during a frequency range (0.4-2.5 Hz). In contrast,
the storage modulus is frequency dependent at low (0.05-0.4 Hz) and high
(2.5-40 Hz) oscillatory frequencies. The stress sweeps showed that the C.
lutea mucilage is characterized by a reversible stress softening behaviour
because the storage modulus decreases at a certain oscillatory stress but it
can reaches its previous value when the stress is removed. These findings
suggest that this mucilage can be used as a rheology modifier for commercial
foods and biomedical materials.

ACKNOWLEDGEMENTS
The authors would like to thank the Peruvian Council of Science and Technology
(Concytec-FONDECYT) and the Vice-Rectorate for Research of the Pontificia
Universidad Catolica del Peru (VRI-PUCP)

REFERENCES
1. Hirst E.L. and Jones J.K.N., The chemistry of plant gums and mucilages.
Journal of the Chemical Society, 56 (1937) 715728.

Polymers from Renewable Resources, Vol. 8, No. 3, 2017 87

Omar P. Troncoso, Bruno Zamora and Fernando G. Torres

2. Kassakul W., Praznik W., Viernstein H. and Hongwiset D., Phrutivorapongkul,

A. and Leelapornpisid P., Characterization of the mucilages extracted from
hibiscus rosa-sinensis linn and hibiscus mutabilis linn and their skin moisturizing
effect. International Journal of Pharmacy and Pharmaceutical Sciences, 6
(2014), 453-457.

3. Hirst E.L. and Jones J.K.N., The analysis of plant gums and mucilages. Modern
Methods of Plant Analysis/Moderne Methoden der Pflanzenanalyse, Berlin
Heidelberg, (1955).

4. Malviya R., Srivastava P. and Kulkarni G.T., Applications of mucilages in drug

delivery-A review. Advances in Biological Research, 5 (2011) 01-07.

5. Prasad Y.R., Krishnaiah Y.S.R. and Satyanarayana S. In vitro evaluation of

guar gum as a carrier for colon-specific drug delivery. Journal of Controlled
Release,51 (1998) 281-287.

6. Franz G., Polysaccharides in pharmacy: current applications and future

concepts.Planta Medica,55 (1989) 493-497.

7. BeMiller J.N., One hundred years of commercial food carbohydrates in the

United States. Journal of Agricultural and Food Chemistry, 57 (2009) 8125-
8129.

8. Kaith B.S., Sharma R. and Kalia S., Guar gum based biodegradable,
antibacterial and electrically conductive hydrogels.International Journal of
Biological Macromolecules,75 (2015) 266-275.

9. Butt M.S., Shahzadi N., Sharif M.K. and Nasir M., Guar gum: a miracle therapy
for hypercholesterolemia, hyperglycemia and obesity. Critical Reviews in Food
Science and Nutrition, 47 (2007) 389-396.

10. Srichamroen, A., Intestinal Transport of Monosaccharides. Naresuan University

Journal, 15 (2007) 127-135.

11. Bhosale R.R., Osmani R.A.M. and Moin A., Natural gums and mucilages:
a review on multifaceted excipients in pharmaceutical science and
research.International Journal of Pharmacognosy and Phytochemical
Research, 15 (2014) 4.

12. Thirupathi K., Kumar S.S., Raju V.S., Ravikumar B., Krishna D.R. and Mohan
G.K., A review of medicinal plants of the genus Cordia: Their chemistry and
pharmacological uses. Journal of Natural Remedies, 8 (2008) 1-10.

13. Basu N.G., Ghosal P.K. and Thakur S., Structural studies on a polysaccharide
fraction from the fruits of Cordia dichotoma Forst.Carbohydrate Research,131
(1984) 149-155.

14. Benhura M.A.N. and Chidewe C., Characterization of the polysaccharide

material that is isolated from the fruit of Cordia abyssinica.African Journal of
Biochemistry Research,5 (2011) 95-101.

88 Polymers from Renewable Resources, Vol. 8, No. 3, 2017

 Thermal and Rheological Properties of the Mucilage From the Fruit of Cordia lutea

15. Haq M.A., Hasnain A. and Azam M., Characterization of edible gum cordia
film: Effects of plasticizers.LWT-Food Science and Technology, 55 (2014)
163-169.

16. Haq M.A., Alam M.J. and Hasnain A., Gum Cordia: A novel edible coating to
increase the shelf life of Chilgoza (Pinus gerardiana).LWT-Food Science and
Technology,50 (2013) 306-311.

17. Haq M.A., Hasnain A., Jamil K. and Haider M.S. Extraction and Characterization
of Gum from Cordia myxa.Asian Journal of Chemistry,26 (2014) 122.

18. Dinda S.C. and Mukharjee B., Gum cordiaA new tablet binder and
emulsifier.Acta Pharmaceutica Sciencia,51 (2009), 189-198.

19. Haq M.A., Alam M.J. and Hasnain A., Gum Cordia: A novel edible coating to
increase the shelf life of Chilgoza (Pinus gerardiana). LWT-Food Science and
Technology, 50 (2013) 306-311.

20. Mayevych I. and Cabanillas J., Chemical composition of Cordia lutea L.:
absence of pyrrolizidine alkaloids. Natural Products Chemistry & Research,
3 (2015) 1-2.

21. El-Mahdy, Rafik A. and El-Sebaiy L.A., Preliminary studies on the mucilages
extracted from Okra fruits, Taro tubers, Jews mellow leaves and Fenugreek
seeds. Food Chemistry, 14 (1984) 237-249.

22. Freanzke L., Lederer A., Malanin M., Eichhorn K., Neinhuis C. and Voig D.,
Plant pressure sensitive adhesives: similar chemical properties in distantly
related plant lineages. Planta, 244 (2016) 145-154.

23. Siddiqui B.S., Perwaiz S., Begum S. and Ali T., Three new constituents,
latifolinal, latifolidin and cordicinol, from the fruits and leaves of Cordia latifolia.
Natural Product Research, 24 (2010) 160-166.

24. Contreras-Padilla M., Rodrguez-Garca M.E., Gutirrez-Cortez E., del

Carmen Valderrama-Bravo M., Rojas-Molina J.I. and Rivera-Muoz E.M.,
Physicochemical and rheological characterization of Opuntia ficus mucilage
at three different maturity stages of cladode. European Polymer Journal, 78
(2016) 226-234.

25. Pawar H.A. and Jadhav P., Isolation, characterization and investigation of
Cordia dichotoma fruit polysaccharide as a herbal excipient. International
Journal of Biological Macromolecules, 72 (2015) 1228-1236.

26. Katzbauer B. Properties and applications of xanthan gum. Polymer Degradation

and Stability, 59 (1998) 81-84.

27. Christianson D.D., Hodge J.E., Osborne D. and Detroy R.W. Gelatinization
of wheat starch as modified by xanthan gum, guar gum, and cellulose gum.
Cereal Chemistry, 58 (1981) 513-517.

Polymers from Renewable Resources, Vol. 8, No. 3, 2017 89

Omar P. Troncoso, Bruno Zamora and Fernando G. Torres

28. Mothe C.G. and Rao M.A. Rheological behavior of aqueous dispersions of
cashew gum and gum arabic: effect of concentration and blending. Food
Hydrocolloids, 13 (1999) 501-506.

29. Bird R.B., Armstrong R.C., Hassager O. and Curtiss C.F. Dynamics of polymeric
liquids, New York: Wiley (1977).

30. Rafe A. and Masood H.S. The rheological modeling and effect of temperature
on steady shear flow behavior of Cordia abyssinica gum. Journal of Food
Processing & Technology, 5 (2014) 1.

31. Rajoria H. and Jalili N., Passive vibration damping enhancement using
carbon nanotube-epoxy reinforced composites. Composites Science and
Technology, 65 (2005) 2079-2093.

32. Bower C., Kleinhammes A., Wu Y. and Zhou O., Intercalation and partial
exfoliation of single-walled carbon nanotubes by nitric acid. Chemical Physics
Letters, 288 (1998) 481-486.

33. Monthioux M., Smith B.W., Burteaux B., Claye A., Fischer J.E. and Luzzi, D.E.,
Sensitivity of single-wall carbon nanotubes to chemical processing: an electron
microscopy investigation. Carbon, 39 (2001) 1251-1272.

34. Torres F.G., Troncoso O.P. Lopez D., Grande C. and Gomez C.M., Reversible
stress softening and stress recovery of cellulose networks. Soft Matter, 5
(2009) 4185-4190.

35. Torres F.G., Troncoso O.P., Rivas E.R., Gomez C.G. and Lopez D., Reversible
stress softening of collagen based networks from the jumbo squid mantle
(Dosidicus gigas). Materials Science and Engineering: C, 37 (2014) 9-13.

36. Storm C., Pastore J.J., MacKintosh F.C., Lubensky T.C. and Janmey P.A.
Nonlinear elasticity in biological gels. Nature, 435 (2005) 191-194.

37. Daas P.J.H., Van Alebeek G.J.W.M., Voragen A.G.J., Schols H.A., Williams P.A.
and Phillips G.O., Gums and Stabilizers for the Food Industry 10 (1999) 318.

38. Benhura M.A.N. and Chidewe C.K., The emulsifying properties of a

polysaccharide isolated from the fruit of Cordia abyssinica. International
Journal of Food Science & Technology, 39 (2004) 579-583.

90 Polymers from Renewable Resources, Vol. 8, No. 3, 2017