Journal of Polymer Research (2018) 25:167

https://doi.org/10.1007/s10965-018-1565-8

ORIGINAL PAPER

Physicochemical and disintegrant properties of sodium Carboxymethyl

starch derived from Borassus aethiopum (Arecaceae) shoot
Shadrack Joel Madu 1,2 & Chukwuemeka Paul Azubuike 1 & Omotunde Okubanjo 1 & Achor Mohammed 3 &
Ochubiojo Martins Emeje 4

Received: 17 September 2017 / Accepted: 29 June 2018

# Springer Nature B.V. 2018

Abstract
Sodium carboxymethyl starch (CMS) samples synthesized from an under-utilized shoot of Borassus aethiopum were
characterized and compared with a commercial brand, sodium starch glycolate. Effects of carboxylation on the physico-
chemical properties of the samples were examined by FTIR, XRD and SEM techniques. The rheological, micromeritics
and disintegrant properties of the samples were also examined. The CMS samples had variable degree of substitution (DS)
with the lowest DS (0.11) comparable to sodium starch glycolate in terms of desirable micromeritics, rheological and
disintegrant properties. FTIR and XRD established modification of the native starch by showing an intense band around
1588 cm−1 to 1608 cm−1 and reduction in the peak intensities for the CMS samples respectively. CMS with variable DS
and desirable micromeritics and rheological properties for potential applications as excipients in biopolymer industries
could be obtained from Borassus aethiopum shoots.

Keywords Borassus aethiopum . Sodium carboxymethyl starch . Physicochemical properties . Micromeritics properties .
Disintegrant

Highlights
• The study established the influence of NaOH concentration and duration
of treatment on degree of substitution of the Borassus aethiopum
carboxymethyl starch.
• Carboxymethyl Starch (CMS) of lower degree of substitution (DS) was
significantly comparable to the standard commercial brand starch (sodi-
um starch glycolate)
• The photomicrograph of the CMS samples showed few alveolate holes
were observed on the surface of the granules which could be attributed to
the strong alkaline environment
• FTIR and XRD confirmed that modification of starch samples led to
decrease in crystallinity.
• Borassus aethiopum carboxymethyl starch had good disintegrant poten-
tial in tablet formulation.

* Chukwuemeka Paul Azubuike 3

Department of Pharmaceutics and Pharmaceutical Microbiology,
cazubuike@unilag.edu.ng Faculty of Pharmaceutical Sciences, Usmanu Danfodiyo University
Sokoto, Sokoto, Sokoto State, Nigeria
1
Department of Pharmaceutics and Pharmaceutical Technology,
Faculty of Pharmacy, University of Lagos, College of Medicine
Campus, PMB 12003, Surulere, Lagos, Nigeria
2 4
Department of Pharmaceutics and Pharmaceutical Microbiology, Centre for Nanomedicine and Biophysical Drug Delivery, National
Faculty of Pharmacy, University of Maiduguri, P.M.B 1069, Institute for Pharmaceutical Research and Development,
Maiduguri, Borno State, Nigeria Abuja, Nigeria
167 Page 2 of 9
Introduction
Starch, an amorphous polymeric carbohydrate made up of an-
hydrous glucose units linked mainly through α-D-(1–4) glyco-
sidic bonds, is a renewable, biocompatible and biodegradable
biomass material. Starch and modified starches have many
industrial applications [1]. It is used as excipients in the food
and pharmaceutical industries (fillers, glidants, thickeners,
binders, disintegrants as well as gelling, bulking, and water
retention agents) [2]. For industrial applications, the choice of
the desired starch product or its modifications is mainly based
on availability and its physicochemical properties, which de-
pends on the source and the processing parameters.
Native starches have limited industrial applications that have
been well documented [3]. Modification of native starches help
to improve their industrial applications and this can be achieved
through chemical, physical or enzymatic processes to provide
desired functional properties for determined uses. Chemical
modification is the most useful way to modify the physicochem-
ical and functional properties of the naturally occurring poly-
mers. Studies and development are now being focused on the
improvement of the known products and synthesis paths as well
as on new derivatives and alternative synthesis concepts [4].
Various studies [5–8] of the carboxymethylation of starch have
been carried out to optimize the reaction conditions (product yield,
reaction efficiency) as well as to improve their functional proper-
ties. Presently, most native and carboxymethylated starches used
as pharmaceutical excipient are sourced from convectional sources
which serve as good sources of nutrition [9], hence, this study was
designed to extract starch from a non-convectional source
(Borassus aethiopum shoot) with limited uses.
The plant Borassus aethiopum (family Aracaceae) was de-
scribed as a palm tree with huge fan shaped leaves [10]. The
young germinating shoot of the plant has aphrodisiac proper-
ties. Fruits and shoot of the plants are the major constituents of
traditional medicine and they also provide the cheapest means
of providing supplies of carbohydrates, fats, protein and min-
erals to the people [10]. The shoots of Borassus aethiopum is
readily available in the northern part of Nigeria with little or no
nutritional value. Some studies have been reported on Borassus
aethiopum shoot starch [11–13]. However, to the best of our
knowledge there is no report on the modification of the
Borassus aethiopum shoot native starch by carboxymethylation
to improve on its functional properties for prospective pharma-
ceutical applications.
Experimental
Materials
Borassus aethiopum shoots were collected on 5th April, 2016
from Hong Local Government Area of Adamawa State, Nigeria.
J Polym Res (2018) 25:167
It was identified and authenticated at Department of Botany,
University of Lagos, Nigeria and a voucher specimen number
LUH 7409 assigned and samples deposited in the herbarium.
Sodium hydroxide (Merck Germany) and sodium
metabisulphate (BDH Chemicals, Pooles, England), Maize
starch B.P., Magnesium stearate powder, Talcum powder,
Paracetamol powder, Lactose and Sodium starch glycolate (were
gift from Phamatex Industries Limited, Lagos, Nigeria). All oth-
er reagents were of analytical grade and were used as received.
Preparation of Borassus aethiopum native
and carboxymethyl starches
Two kg of fresh Borassus aethiopum shoots (BES) was
washed, peeled and allowed to drain for 2 h. The BES were
reduced to about 30 mm and then soaked in water containing
sodium metabisulphate (0.075%w/v) for 24 h prior to pulver-
ization in a mill (TYPE YC100L-4, China). The pulverized
mixture was subsequently stirred and filtered using double
fold clean cheesecloth and then allowed to settle while the
starch sediments. This was followed by decanting the water
and centrifuging the suspension at 4000 rpm for 5 min. The
native starch (BESo) was then air-dried and size-reduced
using porcelain pestle and mortar.
The method employed by Yanli et al., [14] was adopted for
the preparation of Borassus aethiopum carboxymethyl starch
with some modifications. Carboxymethylation was carried
out using ethanol (80%). Sodium hydroxide (0.5, 1.5 and
2.0 M respectively) was mixed with 80 mL of ethanol. The
temperature was maintained at 50 °C and properly stirred until
the NaOH completely dissolved. BESo (10%w/w) was then
poured and stirred vigorously. After stirring, 5 g
monochloroacetic acid (MCA) was added and subsequently
the reaction time varied at 1 h, 2 h and 3 h. After hydrolysis,
the pH of the slurry was adjusted to 7 using 10–20 mL of
glacial acetic acid. The starch was subsequently sieved using
150 mm filter paper with a vacuum pump (TW-1A model,
China), and suspended in methanol. It was sieved again and
the slurry was suspended in 99% ethanol and washed thrice.
The slurry obtained was dispersed in sufficient quantity ace-
tone, stirred for 20 min, and oven dried at 40 °C for 48 h to
obtain samples BESa (0.5 M NaOH, 1 h), BESb (1.5 M
NaOH, 1 h), BESc (1.5 M NaOH, 2 h), BESd (2.0 M
NaOH, 2 h), BESe (1.5 M NaOH, 3 h) and BESf (2.0 M
NaOH, 3 h).
Determination of the degree of substitution
and reaction efficiency of CMS
The method of Lefnaoui, and Mostefa [15] was employed for
determination of DS of the CMS samples while reaction effi-
ciency (RE) was determined by the method of Kweon, and
Bhirud [16].
J Polym Res (2018) 25:167
FTIR spectroscopy
SSG, BESo and Borassus aethiopum CMS samples (5 mg)
were individually blended with solid KBr (50 mg) and com-
pressed into discs. The spectra were scanned from 500 to
4000 cm-1 under dry air at room temperature in a FTIR spec-
trometer (Bruker, South Africa).
XRD study
XRD data were measured at room temperature using a diffrac-
tometer GBC Enhance Mini Material Analyser. The voltage of
35 KV and 35 mA to produce 1225 W and CuKa radiation
(k = 1.54 A°) was set to get an appropriate power for X-ray
source prior to calibration, using pure silicon standard sample.
Samples (5 mg) were then loaded on the sample holder. The
analytical parameters were set to 2o/min using a quartz mono-
chromator, 2θ range 5o to 50o.
Granule morphology
Scanning electron micrographs (SEM) was performed for all
the eight samples with a SEM (Pro X, Netherlands). The sam-
ple starch powders were mixed with ethanol to obtain a 1%
suspension. The suspension (one drop) was then smeared on
aluminum stub with double-sided adhesive tape and the sam-
ple starch powder was coated with gold powder. An acceler-
ating potential of 30 kV was used.
Rheological and related properties
Hydration and swelling capacities
One gram weight of each sample starch powder was weighed
and poured into centrifuge tubes. 10 mL of distilled water was
then added and mixed for 2 min. The mixture was centrifuged
(Micro Centrifugette 4214, Italy) for 10 min at 1000 rpm. The
supernatant obtained was decanted and the sediment weighed
to determine the hydration capacity. Swelling capacity was
determined concurrently with hydration capacity using the
method of Okhamafe et al. [17].
Viscosity
The viscosity of the starch powders were determined using a
digital viscometer (DV-E, China) and the procedure employed
by Nattapulwat et al. [18] was adopted.
Gelatinization temperature
One gram of the powdered sample starch was poured into a
20 mL beaker and 10 mL distilled water added. The dispersion
Page 3 of 9 167
was heated using hot plate. Temperature at which the samples
gel was recorded.
Emulsion capacity and water binding capacity (WBC)
The method used by Omojola et al. [19] was employed for
determination of emulsion capacity while WBC of the starch
powders was assessed using the method described by Sandhu
and Singh [20].
Micromeritics properties
Some micromeritics properties (bulk and tapped densities, an-
gle of repose, powder porosity, Carrs index and Haunser ratio)
as well as moisture content of the starch samples were deter-
mined following the procedures detailed in an earlier study
[21].
Preparation of paracetamol granules
Twelve batches of paracetamol granules were prepared using
wet granulation method. Borassus aethiopum shoot native
starch (BESo), carboxymethylated Borassus aethiopum shoot
starch with the lowest DS (BESa) and the standard sodium
starch glycolate BP (SSG) were employed at concentrations of
2.5, 5, 7.5 and 10%w/w respectively as disintegrant. Weighed
quantities of paracetamol powder and calculated concentra-
tion of intra-granular disintegrant were dry-mixed in a porce-
lain pestle and mortar for five minutes. Subsequently, lactose
was added (as bulking agent when required) separately after
five min of trituration. Maize starch BP paste was added and
mixed to form a damp coherent mass. The coherent mass
formed was passed through number sieve number 1.6 mm to
produce granules. The wet granules were dried in an oven at
40 °C and passed through 1 mm sieve.
Preparation and evaluation of paracetamol tablets
The granules produced were mixed thoroughly with extra
granular excipients (lubricants and glidants) prior to compres-
sion using a single punch tableting machine (Erweka AR 400,
Germany) at uniform compression pressure (8.5 metric tons).
Twelve batches of 100 tablets per batch were produced and
stored in an air tight container for 24 h preceding quality
assessment. Randomly selected tablets from each batch were
evaluated for uniformity of weight, crushing strength and fri-
ability [22].
Disintegration time and dissolution study
The British Pharmacopoeia [23] method was adopted for the
determination of disintegration time and dissolution studies of
the different batches of the paracetamol tablets.
167 Page 4 of 9
Statistical analysis
OriginPro 2016 software (OriginLab Corporation
Northampton, MA 01060 USA) was used for statistical eval-
uation. Mean comparison of the test samples with the standard
was evaluated using one-way analysis of variance. Significant
differences (p < 0.05) were determined by Tukey test.
Results and discussions
Extraction parameters
The yield (29.17%w/w) of the native starch obtained from
Borassus aethiopum shoot is slightly higher than what was
reported by Adamu et al. [11] (23.00%w/w) but lower than
the findings of Muazu et al. [12] (36.85%) and Michel et al.
[13] (35.24%w/w). The variations might be as a result of dif-
ference in processing parameters, botanical source, biological
source, time of collection, age of the plant and also environ-
mental conditions of cultivation [24].
The result of DS of the modified starch samples (BESa,
0.11; BESb, 0.14; BESc, 0.17; BESd, 0.18; BESe, 0.21 and
BESf 0.26) indicates that the DS increased with increase in the
duration of treatment and concentration of NaOH. The in-
creased DS with increasing duration of treatment shows that
adequate time of contact between the starch and the esterifying
reagent can alter the DS. This result is in concordance with the
findings of Yanli et al. [14] and Lefnaoui and Mostefa [15].
According to Vashisht et al. [7], increase in the DS decreases
the percentage release of drug. This further makes the
carboxymethyl derivatives of higher DS a potential excipient
for sustained release formulations.
Increase in the duration of modification and the concentra-
tion of NaOH increased the reaction efficiency during this
study. RE is the fraction of MCA that reacts with starch to
form carboxymethyl starch [25].
FTIR spectroscopy
Although there were some minor differences in some signals
and band intensities, the FTIR spectra of SSG, Borassus
aethiopum shoot native and carboxymethylated starch sam-
ples showed general characteristic spectrum of starch
(Fig. 1). For example, the spectral pattern in the region of
970 and 1200 cm−1 is typical of starch [26], the peaks at
1083 and 1164 cm−1 were observed in all the samples, Li et
al. [27] attributed these bands to the vibration peak of C-O
groups and CH2 symmetrical stretching vibrations respective-
ly and also associated the peaks with the ordered structures of
starch. The intensity of bands at the two peaks were more
pronounced in the native starch than in the carboxymethylated
samples indicating that the carboxymethylated samples were
J Polym Res (2018) 25:167
more amorphous. Another striking difference in the spectra of
the starch samples was the intense band at around 1588 to
1608 cm−1 for CMS samples attributed to carbonyl functional
group (the peaks of CMS with higher DS were obvious thus
confirming functional group modification) while the native
starch had band at 1655 cm−1 assigned to the scissoring of
two O-H bonds of water molecules [27]. A more detailed
description of the FTIR spectrum of starch and CMS has been
reported [27].
XRD study
The XRD patterns for SSG, BESo, and the Borassus
aethiopum shoot CMS samples are presented in Fig. 2.
Borassus aethiopum shoot native and CMS samples X-ray
diffractograms showed two strong reflections at approximate-
ly 17. 3 and 23.6 ° 2θ while that of SSG appeared at 17.4 and
24.5° 2θ. The X-ray diffraction pattern of the starch samples is
a characteristic pattern of A type crystallinity for native starch
as reported in previous study [25]. However, there were de-
crease in the peak intensities for the CMS samples. The reduc-
tion in the peak intensities might be attributed to the reduction
in the crystallinity of the samples as a result of
carboxymethylation. The loss of crystallinity in
carboxymethylated starches was not unanticipated, consider-
ing the extensive granule distortion, observed with SEM. As a
result of anticipated increase in solubility due to higher pro-
portion of amorphous portion, tablet disintegration can be en-
hanced if wicking is considered as the mechanism of disinte-
gration when the CMS samples are employed as disintegrant.
Granule morphology
The SEM photomicrographs of the SSG, native and
carboxymethylated Borassus aethiopum shoot starch sam-
ples are presented in Fig. 3. The granules of the native
starch surfaces appeared smooth, oval, shell and ellipsoid
shaped and the sizes were smaller compared to those of
carboxymethylated samples. The arrangement is consistent
with the findings of Muazu et al. [12]. As observed from
the SEM photomicrographs, carboxymethylation of the na-
tive starch led to significant alterations of the granular
structure of the native starch. Few alveolate holes were
observed on the surface of the granules of CMS samples
and there were minor differences in the photomicrographs
among various CMS samples. The differences could be
attributed to the strong alkaline environment the starch
samples were subjected to during carboxymethylation
[14]. It is reasonable that the strong alkaline condition
caused granular disintegration. These differences in parti-
cle shape, size and distribution might have effect on the
functional properties of the powders when employed as an
excipient in formulations.
J Polym Res (2018) 25:167 Page 5 of 9 167

1.08

BESb

BESf
0.90
0.81

0.72
0.54

0.54
0.27

0.36
0.00
BESa
0.90

BESe
0.95

0.72 0.76

0.54 0.57
Transmittance

0.36 0.38
BESo

Transmittance

BESd
0.90 0.87

0.75 1655 0.58

0.60 0.29

0.00
0.95
SSG

BESc
0.90
0.76
0.75
0.57
0.60
0.38

4000 3500 3000 2500 2000 1500 1000 500 4000 3500 3000 2500 2000 1500 1000 500

Wavenumber (cm-1) Wavenumber (cm-1)

Fig. 1 Stacked FTIR spectra of SSG, BESo and Borassus aethiopum shoot CMS (BESa to BESf) samples. The solid vertical lines indicate some
important signals characteristic of starch based samples while dashed lines indicate signal characteristic of CMS samples

Rheological properties samples might be attributed to the addition of negatively

Some rheological properties of the native and
carboxymethylated starch powders are presented in Table 1.
Generally, carboxymethylation of the native starch led to in-
crease in hydration capacity of the samples. However, the
hydration capacities of CMS samples were significantly lower
than that of SSG. The hydration capacities of the CMS
BESb
charged carboxymethyl group. Similarly, swelling power of
the CMS powders increased with starch modification. The
swelling powers of the CMS samples were found to be signif-
icantly better than that BESo but less than that of SSG. This
might be due to water penetrating into the starch granules as a
result of the hydrophilic nature of carboxymethyl groups.
Higher swelling and hydration capacities had been reported

39.2
25.2
29.4
BESf

18.9
19.6
12.6
9.8
26.4 6.3
BESa

19.8 22.4
BESe

13.2 16.8

6.6 11.2

52 5.6
BESo
Counts

39 24
BESd
Counts

26 18

13 12

34.0 31.6
SSG

BESc

25.5 23.7

17.0 15.8

8.5 7.9
5 10 15 20 25 30 35 40 45 50 5 10 15 20 25 30 35 40 45 50
2 Theta(o) Theta(o)

Fig. 2 Stacked XRD patterns of SSG, BESo and Borassus aethiopum shoot carboxymethylated starch (BESa to BESf) samples. The solid vertical lines
indicate some important signals characteristic of starch based samples
167 Page 6 of 9 J Polym Res (2018) 25:167

Fig. 3 SEM photomicrographs of SSG, BESo and the carboxymethyl starch (BESa to BESf) samples

to have significant effects on the disintegrant properties of
starches [1], hence the CMS samples might be good
disintegrant when employed in pharmaceutical formulations.
The viscosities of the CMS powders, native starch, and
SSG were found to be statistically different. Unlike reported
in a previous study [18], there were no correlation between the
degree of substitution and viscosity obtained from the study.
However, most of the CMS samples with higher DS were
more viscous. The high viscosity of the CMS samples with
higher DS had been attributed to more water penetrating into
the starch granules due to the hydrophilicity of the
carboxymethyl groups [18] hence, the CMS samples could
be good suspending agents.
Gelatinization temperature of SSG (54.90 °C) was signifi-
cantly lower than that of BESo (65.00 °C) while those of
Borassus aethiopum shoot CMS samples varied from 52 to
64 °C. Generally, the temperature decreased with
carboxymethylation of the native starch. Sasaki [28] reported
that starch with higher amylose content was more amorphous
and less crystalline with lower gelatinization temperature and
endothermic enthalpy. The lower gelatinization temperature of
the CMS samples correlated to the more amorphous nature of
the samples reported in the X-ray study. The emulsion capac-
ity of SSG (13.33%) was significantly higher than that of
BESo (9.33%). The CMS samples were significantly higher
(10.00–14.00) in emulsifying capacities than the native starch

Table 1 Rheological properties of the starch powders

Starch Hydration capacity Swelling capacity Viscosity (mPa.s) Gelatinization Emulsion capacity WBC
Samples temperature (°C) (%)

SSG 10.23 ± 0.12 692.31 ± 0.26 101.50 ± 4.35 54.90 ± 1.47 10.36 ± 0.00 10.36 ± 0.00
BESo 1.90 ± 0.80 6.67 ± 0.25 107.50 ± 6.17 65.00 ± 0.79 9.33 ± 0.27 0.78 ± 0.07
BESa 1.83 ± 0.16 7.14 ± 0.15 114.00 ± 2.84 64.00 ± 0.01 11.55 ± 0.52 2.15 ± 0.07
BESb 3.10 ± 0.08 75.00 ± 0.10 88.50 ± 2.64 57.10 ± 0.10 10.00 ± 0.00 3.34 ± 0.06
BESc 3.34 ± 0.23 87.50 ± .26 109.00 ± 5.10 52.00 ± 0.01 10.00 ± 0.00 3.34 ± 0.06
BESd 5.25 ± 0.39 150.00 ± 1.06 157.00 ± 5.22 47.00 ± 2.10 14.00 ± 0.09 4.55 ± 0.07
BESe 3.34 ± 0.12 118.75 ± 0.22 129.50 ± 14.42 53.96 ± 1.00 13.33 ± 0.77 2.70 ± 0.14
BESf 5.15 ± 0.04 200.00 ± 1.00 109.50 ± 2.05 56.00 ± 0.20 12.00 ± 0.46 6.73 ± 0.23

SSG, sodium starch glycolate; BESo, native Borassus aethiopum shoot starch; BESa to BESf, Borassus aethiopum shoot CMS starch; WBC, water
binding capacity
J Polym Res (2018) 25:167 Page 7 of 9 167

thus indicating the chemical modification gave a better emul-
sifying property.
The water binding capacity (Table 1) of SSG was signifi-
cantly higher than those of BESo and the CMS. The water
binding capacities of BESa to BESf increased slightly with
increase in DS indicating variation in the proportion of crys-
talline and amorphous regions within the granules of the of the
modified starch samples of various DS [29]. This attribute
might also play an important role in tablet disintegration when
employed as disintegrant.
Micromeritics properties
The results of some micromeritics properties are presented in
Table 2. Generally, the bulk and tapped densities of Borassus
aethiopum shoot CMS samples were significantly less than
that of SCG and BESo. However, there was no significant
difference in the bulk density between SSG, BESo, BESa
and BESc while for tapped density the standard starch, native
starch and BESa demonstrated no significant difference. This
could be attributed to the change in granular structure/
crystallinity of the powder during chemical modification
which could affect the starch powder property [30]. The sam-
ples with lower DS also showed higher bulk and tapped den-
sities compared to those samples with higher DS. The impli-
cation of this is the likelihood of the lower DS having a better
flow compared to those samples with higher DS since higher
bulk and tapped densities are associated with better flow prop-
erties [21]. The suggestion of better flow properties for the
native and CMS with lower DS samples is also supported by
the results of Carr’s index and Hausner’s ratio of the samples.
The unmodified starch and SSG had Carr’s index of 19.54 and
18.61 while the Hausner’s ratios were 1.24 and 1.23 respec-
tively. Carr [31] had classified the flow property of powder
using Carr’s index. According to the classification, values of
the index in the ranges of 5 to 10, 12 to 16, 18 to 21 and 23 to
28 indicate excellent, good, fair and poor flow characteristics
of a powder material respectively. Based on the classification,
SSG, BESo and BESa (DS; 0.11) could be classified as pow-
ders with fair flow properties while other CMS samples had
poor flowability. Similarly, for Hausner’s ratio, value of less
than 1.20 indicates good flowability while value of 1.5 or
higher suggests poor flow properties [32]. In this study, those
ratios for SSG, BESo and BESa lie around the threshold of
1.20 whereas other CMS samples were 1.55 and above indi-
cating very poor flow properties. However, results of angles of
repose (Table 2) are not fully consistent with those of Carr’s
index and Hausner’s ratio. The result for angle of repose indi-
cates that the native starch had a reasonable flow unlike re-
ported for Carr’s index and Hausner ratio [33]. It is worthy to
note that angle of repose is sensitive to moisture content of
powder samples [34]. Reduction in the residual moisture con-
tent by drying might significantly improve the flow property
of the CMS starch samples [35].
The moisture content of the samples is presented in Table 2.
Several Pharmacopeias have set a limit for their moisture con-
tents to be 15.0% [36]. Based on this, the native starch, BESa
and SSG had their moisture contents within the limit while
other CMS samples were within the threshold or more than the
stated limit.
The porosities of Borassus aethiopum shoot CMS samples
(Table 2) were found to be significantly higher than those of
SSG and BESo. The differences might be explained by the
fact that the powders have a wide range of particle sizes and
shapes. The result of SEM photomicrographs of the starch
samples is consistent with the porosity values.
Physical properties of the paracetamol tablets
The results of the physical properties of the tablets produced
using different concentrations of the starches as disintegrant
are presented in Table 3. From the result of uniformity of

Table 2 Some Micromeritics Properties of the starch samples

Starch Bulk density Tapped density Angle of repose Carr’s index Hausner’s ratio Powder porosity Moisture content
Samples (g/mL) (g/mL) (θ°) (%)

SSG 0.70 ± 0.02 0.86 ± 0.03 40.90 ± 1.21 18.61 ± 0.05 1.23 ± 0.07 3.18 ± 0.15 14.56 ± 0.45
BESo 0.70 ± 0.01 0.87 ± 0.12 24.55 ± 0.72 19.54 ± 0.10 1.24 ± 0.14 3.03 ± 0.15 11.81 ± 0.20
BESa 0.63 ± 0.01 0.80 ± 0.04 31.60 ± 0.00 21.25 ± 0.04 1.26 ± 0.04 4.35 ± 0.08 12.49 ± 0.08
BESb 0.43 ± 0.02 0.67 ± 0.08 48.51 ± 2.36 35.82 ± 0.09 1.55 ± 0.22 7.50 ± 0.17 15.21 ± 0.25
BESc 0.46 ± 0.01 0.71 ± 0.03 46.25 ± 0.60 35.21 ± 0.04 1.54 ± 0.10 7.60 ± 0.40 14.92 ± 0.57
BESd 0.37 ± 0.05 0.60 ± 0.05 47.55 ± 0.35 38.33 ± 0.03 1.62 ± 0.13 10.50 ± 0.39 19.57 ± 1.39
BESe 0.46 ± 0.03 0.66 ± 0.09 45.62 ± 0.29 30.30 ± 0.09 1.43 ± 0.21 8.18 ± 0.61 15.24 ± 0.20
BESf 0.34 ± 0.09 0.59 ± 0.06 46.64 ± 0.64 42.37 ± 0.16 1.73 ± 0.87 4.23 ± 0.87 18.03 ± 0.43

SSG, sodium starch glycolate; BESo, native Borassus aethiopum shoot starch; BESa to BESf, Borassus aethiopum shoot CMS starch; WBC, water
binding capacity
167 Page 8 of 9 J Polym Res (2018) 25:167

Table 3 Properties of tablets

formulated with different Starch Uniformity of Crushing Friability test Disintegration % Dissolved
disintegrants Samples weight (g) strength (Kg) (%) time (sec) at 30 min

SSGT 1 0.61 ± 0.01 8.54 ± 3.58 0.31 ± 0.00 69.60 ± 1.80 73.80 ± 0.03
SSGT 2 0.63 ± 0.00 11.92 ± 0.47 0.78 ± 0.15 13.80 ± 3.00 76.31 ± 0.05
SSGT 3 0.62 ± 0.00 5.64 ± 0.29 0.80 ± 0.13 12.60 ± 1.80 74.34 ± 0.00
SSGT 4 0.64 ± 0.00 5.14 ± 0.86 0.46 ± 0.05 18.60 ± 2.40 76.05 ± 0.16
BESo T 1 0.63 ± 0.01 15.02 ± 0.16 0.95 ± 0.04 722.40 ± 511.8 60.33 ± 0.09
BESo T 2 0.63 ± 0.00 12.28 ± 0.76 0.94 ± 0.02 30.00 ± 1.80 65.54 ± 0.04
BESo T 3 0.63 ± 0.01 15.16 ± 0.08 0.63 ± 0.03 91.20 ± 52.8 63.08 ± 0.45
BESo T 4 0.62 ± 0.01 4.40 ± 0.65 0.34 ± 0.00 11.40 ± 1.80 68.45 ± 0.32
BESa T 1 0.63 ± 0.00 8.70 ± 0.57 0.79 ± 0.11 54.00 ± 30.00 87.61 ± 0.00
BESa T 2 0.63 ± 0.00 7.28 ± 0.25 1.20 ± 0.23 33.60 ± 0.00 78.03 ± 0.36
BESa T 3 0.64 ± 0.00 5.12 ± 0.10 0.77 ± 0.06 24.60 ± 6.60 80.81 ± 0.11
BESa T 4 0.64 ± 0.00 4.04 ± 0.11 2.27 ± 0.10 19.80 ± 9.00 83.05 ± 0.47

*where 1, 2, 3 and 4 represents the percentage weight by weight disintegrant concentration and T = tablet; All the
data for each parameter represented the average of three (3) analysis ± standard deviation (SD)

weight, the range of deviation of the tablets for the whole
batches produced were within the range of 0.00–0.01. This
implies that the tablets have less than 5% deviation as permit-
ted for tablets weighing more than 250 mg according to BP,
[23]. Similarly, it also complies with the USP, [37] specifica-
tion that none of the tablets should be more than 324 mg
compared to the others if the tablets are weighing more than
250 mg. The crushing strength of all the batches formulated
was found to be above the minimum requirement for a satis-
factory tablet (a force of about 4 kg) (38). There was statisti-
cally significant difference between the batches containing
SSG as disintegrant and all the other batches P < 0.05. In
addition, with increasing disintegrant concentration, the
crushing strength of the tablets decreases.
The tablets formulated were within the specification of
the USP (37) for friability test (< 1%), however, BESo T 1,
BESo T 2, BESa T 2 and BESa T 4 failed the requirement
of the BP [23] by exceeding the upper limit 0.8%. This
implies that the physical integrity of tablets formulated
can be conserved when exposed to factors that are not se-
vere enough to break the tablet, but may abrade small par-
ticle from tablet surface (for example; during coating, pack-
aging and transport) [38].
The disintegration time for tablets formulated with SSG
as disintegrant was significantly lower than those formu-
lated with BESo and BESa. Disintegration time for tablets
formulated with BESa as disintegrant were generally lower
than those formulated with the native starch. This implies
that carboxymethylation increased the disintegrant poten-
tial of the starch. The lower disintegration time obtained
for tablets formulated with the Sodium starch glycolate
might be attributed to the difference in modification con-
ditions as well as the source of the starch. This observed
difference correlated with the findings reported earlier un-
der the XRD, granular morphology as well as rheological
studies. However, all the batches of the paracetamol tablets
disintegrated in less than 15 min, hence they complied with
the BP [23] specification with respect to tablet disintegra-
tion for uncoated tablets. Generally, the disintegration time
also decreases as the concentration of disintegrant was in-
creased as reported by Vashisht et al., [7] and Das et al.,
[39].
The dissolution data (Table 3) of the paracetamol tablets
formulated with SSG and BESa as disintegrant showed that
the tablets released more than 70% of the active drug at
30 min, while those formulated with the native starch did
not. Hence, the tablets formulated with the carboxymethylated
starches as disintegrant passed the official dissolution specifi-
cation [23].
Conclusion
Modification of the native Borassus aethiopum shoot starch
led to the production of CMS samples with varying DS as well
as desirable and unique physicochemical properties for poten-
tial applications as excipients in pharmaceutical formulations.
Overall, modified starch sample with lowest DS was compa-
rable to commercial brand, sodium starch glycolate mainly in
terms of rheological, micromeritics and disintegrant properties
and might be potential source of less expensive excipient for
immediate release formulations.
Compliance with ethical standards
Conflict of interest None.
J Polym Res (2018) 25:167
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