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Thermal and Rheological Properties of The Mucilage From The Fruit of
Thermal and Rheological Properties of The Mucilage From The Fruit of
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.
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;
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
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 4°C. 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
110°C to remove all the evaporable compounds and then cooled at 30°C for
5 minutes. Dry samples were heated from 30°C to 400°C with a heating rate
of 3°C/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 30°C to 220°C using a
heating rate of 10°C/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
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 25°C 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 25°C and 1 Hz,
respectively. A minimum of 5 samples extracted from 5 different C. lutea fruits
were used per condition.
Figure 2. FTIR spectrum of the mucilage extracted from the fruit of C. 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
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
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 158°C. 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)
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