Isolation, Characterization,
Evaluation and Establishment of Polymeric Principles from Curcuma Angustifolia as Multitasking Excipient
Anshita Gupta*
Shri Rawatpura
Sarkar Institute of Pharmacy, Kumhari, Durg
*Corrosponding
author: dr.anshitasoni@gmail.com
[Received: 30 January 2019; Revised
version: 16 March 2019; Accepted: 28 March 2019]
Abstract.
In
India, Chhattisgarh is famous as Herbal state with its beautiful natural
resources of forests and agricultural fields and value addition has been done
so far in Chhattisgarh to maintain or improve the quality of the plants before
the material reaches the industry. Presently, the herbal industry in
Chhattisgarh is not very organized. The plant
derived gums, mucilages from natural sources
like carrageen an, thaumatin, lard, storax, agar, gum acacia, tragacanth and
many more to name comply with many requirements of pharmaceutical excipients.
These can be preferred for formulation development as being stable and
involving less regulatory issues as compared to their synthetic counter parts.
They can also be easily modified to meet the specific needs, thereby being a
potent and economic vehicle for delivering active pharmaceutical ingredient in
formulation. Thus our concerned and aims of the study is to throw light on the
potential of natural excipients which can be proposed to be used as diluent,
binder, disintegrant as well as lubricant in various types of formulations as
they are biocompatible and capable of giving additional nutrition to the
developed dosage form from indigeneous sources of Chhattisgarh state which
could serve for cost effective and economical medicament and will enhance the
value addition to the proposed herb and herbal species.
Key Words: herbal state, diluent, binder, disintegrant, excipients, active
pharmaceutical ingredient.
Introduction
In India, Chhattisgarh is famous
as Herbal state with its beautiful natural resources of forests and
agricultural fields and value addition has been done so far in Chhattisgarh to
maintain or improve the quality of the plants before the material reaches the
industry. Presently, the herbal industry in Chhattisgarh is not very organized.
(Kokate et al., 1994) Through the state lead initiatives on In-situ
conservation, Ex-situ cultivation and propagation, capacity building of local
communities, development of processing technologies and emphasis on value
addition on herbal product. In the same lieu arrives the demand and necessity
of natural excipients from herbal origin to produce cost effective,
standardized, biocompatible and safe drugs. Excipients play a critical role in
the creation of medicines, helping to preserve the efficacy, safety, and
stability of active pharmaceutical ingredients (APIs) and ensuring that they
deliver their promised benefits to the patients. Optimal use of excipients can
provide pharmaceutical manufacturers with cost-savings in drug development,
enhanced functionality and help in drug formulations innovation. (Kokate et al., 1994; Patel et al., 2015)] Thus our concerned and aims of the study is to throw light on
the potential of natural excipients which can be proposed to be used as
diluent, binder, disintegrant as well as lubricant in various types of
formulations as they are biocompatible and capable of giving additional
nutrition to the developed dosage form from indigeneous sources of Chhattisgarh
state which could serve for cost effective and economical medicament and will
enhance the value addition to the proposed herb and herbal species.
Materials and
Methods
Tikhur rhizome
was procured from the local market of jagdalpur Chhattisgarh and extracted for
starch as mentioned by the procedure of Patel et al. (2015). Extracted starch
was used for evaluation of physico chemical and different excipient properties
(Patel et al., 2015).
Chemical
composition Moisture, crude protein, crude fat and ash content were determined
using AACC (2000) standard methods. Starch content in tikhur was determined
using IS 4706-2 (BIS, 1978) method. Amylose content in tikhur was measured by
the procedure reported by and amylopectin content was calculated using Eq. (1).
Amylopectin% = 100 – amylose%
Swelling index
Swelling characteristics swelling
characteristics of the starches were studied at different temperatures by
microscopic method. The extend of swelling was calculated by finding the ratio
between grain size at the maximum temperature and at 35°C (Kumari et al., 2012)
Paste clarity
Paste clarity (%
Transmittance at 640 nm) of starch paste was measured using the procedure of
Craig et al. (1989). Starch suspension (2%) was heated and stirred in water
bath for 30 min at 95 °C. Samples were cooled and stored for 4 d at 4 °C and
percent transmittance was measured everyday at 640 nm against water blank using
UV – VIS Spectrophotometer (Kumari et al., 2012).
Pasting properties
Pasting properties of
tikhur flour were measured using Rapid Visco-Analyser 4D (RVA) manufactured by
M/s Newport Scientific Pvt Ltd., Australia, according to the method described
by Yadav et al. (2010). 3.5 g of flour sample with an initial moisture content of 2.63%
(wet basis) was dispersed in 25 ml of distilled water and fitted into RVA as
per manufacturer’s instructions. The rotating speed of paddle was 160 rev/min
except for first 10 sec (960 rev/min). The suspension was equilibrated at 50 °C
for 1 min and heated at the rate of 12 °C/min to 95 °C and then held at 95 °C
for 2.5 min. The sample was then cooled to 50 °C at the rate of 12 °C/min and
then held for 3 min at 50 °C. Peak viscosity, trough viscosity, breakdown
viscosity, final viscosity and setback viscosity were recorded in rapid
viscosity units (RVU). Pasting temperature (°C) was also recorded and test was
replicated thrice (Rani et al., 2012; United State Pharmacopoeia, 1985).
Gel strength
Tikhur starch suspension (prepared
with a concentration of 8% starch solids, (db) was heated to 95 °C and held for
30 min and cooled to 4-6 °C for gel formation; Gel strength was determined
using Texture Analyzer (TA XT CT 3 Model). The following conditions were used
for measurement of gel strength of tikhur starch: pre-test speed: 3.0 mm/s;
test speed: 2.0 mm/s post-test speed: 10.0 mm/s; distance: 15 mm; trigger type:
Auto – 15 g; data acquisition rate: 400 pps. For gel strength measurement, when
a trigger force of 15 g was attained the probe then proceeded to penetrate into
the gel at a speed of 2.0 mm/s to a depth of 15 mm. During this penetration,
the force was seen to drop at the point where the gel broke thrice (Rani et
al., 2012; United State Pharmacopoeia, 1985). Thereafter, the resulting forces
were due to continuing penetration up to the required depth. Hardness or gel
strength, deformation at target and adhesiveness were obtained through this
measurement.
Fourier transform-infrared spectroscopy
Fourier transform infrared spectroscopy
(Nicolet-6700, ThermoFisher, United States) was used to determine the
functional groups in the wave length range of 4000–400 cm−1 of starch samples.
Before taking FT-IR, the sample was blended with KBr (Indian Pharmacopoeia,
1966)
Bulk density
Bulk density (Db) It is ratio of
total mass of powder to the bulk volume of powder. 10 gm of drug excipient
mixture were taken and transferred into a 50 ml measuring cylinder and the
volume was noted. The bulk density of the powder were expressed in gm/ml was determined
as follows.
Db = M/Vo
Where, M is the mass of the powder Vo is the bulk
volume of the powder.
Scanning electron
microscopy
Scanning Electron Microscopy (SEM)
is generally used to characterize starch at microstructure level. The
results obtained by SEM showed variation in size and shape of starch granules
from small to large and oval to polyhedral with the size ranging from 9.75 to
20.43 µm in length and 3.409 to 5.272 µm in width (Nakhat et al., 2004).
Rheological studies
Rheological studies of Starch
mucilage Starch mucilage (5% and 10%) of Curcuma angustifolia were prepared.
The rheological characteristic of mucilage was evaluated by using Brookfield
viscometer (Perez et al., 2015).
Angle of repose
The frictional forces in a loose
powder can be measured by the angle of repose, q. This is the maximum angle
possible between the surface of a pileof powder and the horizontal plane and it
is given as, tan q = h / r,
q = tan-1[h /r]
Where q is the angle of repose, h is the height in
cm, r is the radius.
The powder mixture was allowed to
flow through the funnel fixed to a stand at definite height. The angle of
repose was then calculated by measuring the height and radius of the heap of
powder formed.
Test for friability and flow properties of granules
Paracetamol granules prepared with
Curcuma angustifolia starch and Corn starch were tested for friability and flow
properties [9]. Friability testing was carried out using Roche friabilator.
Friability was calculated from the following formula
%
Friability = (1-W1/W2) x 100
Where, W1 = weight of
granules after test. W2 = weight of granules before test. Flow properties of
granules were tested by determining angle of repose.
Statistical data analysis
Experiments were performed three
times, and data were analyzed by one sample t-test analysis to determine
significant differences at p < 0.05 using SPSS 16.0 statistical software
(SPSS, Inc., Chicago, IL, USA).
Evaluation and
establishment of herbal excipient-based formulation (of tablets)
Hardness and friability tablets
Hardness and
Friabilator testing were carried out by using Monsanto hardness tester and
Roche friabilator respectively.
Uniformity of weight
The weight variation
test of the tablets was performed as per I.P. Twenty tablets of each type were
weighed and average weights were calculated (Patel et al., 1994; Nakhat et al.,
2004).
Thickness of tablets
The thickness of six tablets was
measured using Vernier calipers. The extent to which the thickness of each
tablet deviated from ± 5% of the standard value was determined. Six tablets
from each batch were selected and evaluated, and the average value with
standard deviation was recorded (Indian Pharmacopoeia, 1996).
Disintegration Test
All the six formulations were
tested for disintegration time as per method prescribed in I.P. for uncoated
tablets. Assay Assays were carried out by using the method prescribed in I.P.10.
Dissolution studies
Dissolution studies
were performed as per procedure given in I.P10. The sampling time specified in
I.P. The sampling time specified in I.P. was modified instead of withdrawing a
single sample after 30 minutes; serial sampling was done at 5, 10,15,20,25 and
30 minutes (Indian Pharmacopoeia, 1996).
Results and Discussion
Physical and chemical characteristics
Physicochemical properties of
tikhur starch are presented in Table 1.The average grain size, loss on drying,
pH, ash value and angle of response is shown in the table. Swelling
characteristics of the starches were studied at different temperatures by
microscopic method (Table 2). The extend of swelling was calculated by finding
the ratio between grain size at the maximum temperature and at 35°C. Grains of
Curcuma angustifolia starch were found to be smaller in size than of Corn
starch. They were round, granular in shape. Not much difference was observed in
loss on drying, acidity, ash value, pH values of Curcuma angustifolia starch
and Corn Starch. The loss on drying and acidity values was well within official
limit Table 1. The bulk density, angle of repose and compressibility index of
both starches was comparable.
|
Table
1. Physicochemical properties of tikhur starch
|
|
S.No.
|
Properties
|
Tikhur
Powder
|
Corn
Starch
|
|
1.
|
Average
Grain size (micron)
|
11.86±0.21
|
23.48
±0.15
|
|
2.
|
Loss
on Drying (%)
|
10.46±0.3
|
10.01±0.27
|
|
3.
|
Acidity
(ml of 0.01 M NaOH)
|
0.4
|
0.43
|
|
4.
|
pH
|
6.22
|
6.35
|
|
5.
|
Ash
Value (%)
|
0.260±0.17
|
0.300±0.21
|
|
6.
|
Bulk
Density (g/c/c)
|
0.65±0.25
|
0.55±0.28
|
|
7.
|
Angle
of repose (Degree)
|
28.35
|
35.34
|
|
*Corn
Starch Taken as Reference, **Tikhur is scientifically known as Curcuma
angustifolia powder
|
|
|
|
|
|
|
|
Table
2. Swelling
characteristics of the starches at different temperature
|
|
S.No.
|
Temperature(°C)
|
Tikhur Powder
|
Corn Starch
|
|
|
1.
|
35
|
9.86±0.31
|
23.48±0.16
|
|
|
2.
|
40
|
10.13±0.11
|
24.02±0.22
|
|
|
3.
|
50
|
12.88±0.14
|
25.31±0.14
|
|
|
4.
|
60
|
14.45±0.25
|
26.92±0.11
|
|
|
5.
|
70
|
16.67±0.21
|
38.37±0.27
|
|
|
6.
|
80
|
17.21±0.39
|
47.68±0.24
|
|
|
7.
|
Swelling Ratio
|
2.198±0.18
|
2.023±0.13
|
|
Bulk density is
a measure of heaviness of solid samples, which is important for determining
packaging requirements, material handling and application in the pharmaceutical
as well as food industry (Singh et al., 2011). Bulk density of tikhur starch is
quite lesser than (0.65g/cc) Wheat flour (0.73g/cc). Tikhur starch is not
suitable as thickener in food products as it is recommended that flours with
high bulk densities (> 0.7 g/mL) are used as thickeners in pharmaceuticals
(Akubor and Badifu 2004; Falade and Okafor, 2015).
|
Table 3. Hardness
and % friability of the tablets
|
|
Product
|
Friability (%)
|
Hardness (Kg/sq.cm)
|
|
|
Paracetamol Granules
|
|
|
|
|
|
|
Tikhur Powder
|
0.692 ±0.025
|
3.50±0.325
|
|
|
|
|
|
Corn Starch
|
0.520± 0.056
|
3.50±0.436
|
The friability testing of granules
showed that the Corn starch had slightly high binding strength than that of
Curcuma angustifolia starch Table 3.
|
Table 4. Uniformity of Tablets
|
|
Product
|
Average
weight
|
Maximum
deviation
(%)
|
Assay
(Percent of
labeled amount)
|
|
Paracetamol Tablets
|
|
Tikhur Powder
|
620
|
+2.8
|
99.7%
|
|
|
|
-3.5
|
|
|
Corn Starch
|
620
|
+3.6
|
100.25%
|
|
|
|
-2.5
|
|
In all the cases the values of
angle of response were ≤30°, which indicate that both the starches were free
flowing. Hardness and % friability of the tablets were found to be well within
acceptable limits Table 3. It showed that Curcuma angustifolia starch may
exhibit good disintegrating property over corn starch. This disintegrating
property may be attributed to the more number
of starch grains per mg of sample.
|
Table
5. disintegration time of paracetamol (tablets (n=6)
|
|
Product
|
% Disintegrant
|
Disintegration
Time
|
|
|
|
(Sec.)
|
|
|
Paracetamol
tablets
|
|
|
Tikhur
Powder
|
10.0
|
145±2.012
|
|
|
5.0
|
|
|
|
2.5
|
215±1.784
|
|
|
|
355±3.462
|
|
Corn
Starch
|
10.0
|
154±1.036
|
|
|
5.0
|
260±2.565
|
Scanning electron
microscopy
Scanning Electron Microscopy (SEM)
is generally used to characterize starch at microstructure level. The
results obtained by SEM showed variation in size and shape of starch granules
from small to large and oval to polyhedral with the size ranging from 9.75 to
20.43 µm in length and 3.409 to 5.272 µm in width.
Figure
1. Scanning electron microscopy of Tikhur Powder
Water absorption characteristics
represent the ability of a product to associate with water under conditions
where water is limiting. The water and oil absorption capacity of tikhur starch
was 2.32 + 0.18 g/g and 1.92 + 0.04 g/g respectively. The maximum water
absorption was about 40% for starches. Higher water absorption of starch helps
in maintaining water soluble delivery system. Oil absorption capacity reflects
the emulsifying capacity. The correlation coefficient between water and oil
absorption capacity was 0.29 stipulating that amylose can form complexes with
lipids also.
Paste clarity
Clarity is a key parameter in
starch paste quality because it gives shine and opacity to product
colour. Percent transmission of tikhur starch decreased gradually from 54.6 to
50.4% on 4 th day. Decrease in light transmittance of starch pastes with the
increase in storage time is attributed to recrystallization of starch (Shah et
al., 2016). But it is generally higher than percent transmittance of cassava
(50.6%) and potato starch (42.2%) as outlined by Nuwamanya et al. (2011)
Gel Strength
A number of factors
have been suggested to be responsible for the strength of starch paste.
Intrinsic interaction of the starches which is governed by their relative
hydrophilicity/hydrophobicity, ability to form complex, relative content of
amylose/amylopectin, rearrangement of the amylose chains which led to increase
in the porosity of the matrix and presence of nonstarch polysaccharides which
may hinder hydrogen bond formation could affect the paste strength.
Conclusion
Tikhur is a unique starch with
therapeutic benefits suitable for use in different sweets as it imparts no
after taste. The medium amylose content, clarity and good solubility in water.
There is an excellence scope for Curcuma angustifolia starch. Hence newer natural
substance must be studied for its pharmaceutical application. Curcuma
angustifolia starch could be used as a promising pharmaceutical excipient in
tablet technology as, it showed adequate binding and disintegrating properties.
Acknowledgement
Author
wants to thanks the Dr.Chanchal Deep Kaur, Principal SRIP, Kumhari for
providing necessary facilities to carry out the work.
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