Evaluation of compatibility between dried extracts of Myracrodruon urundeuva Allemão and pharmaceutical excipients by TG and DTA
J Therm Anal Calorim
Evaluation of compatibility between dried extracts of Myracrodruon urundeuva Allem a˜o and pharmaceutical excipients by TG and DTA
Renata da Silva Leite 0 1
Valmir Gomes de Souza 0 1
Islaine de Souza Salvador 0 1
Agna He´lia de Oliveira 0 1
Ant oˆnio de Lima Neto 0 1
Ionaldo Jose´ Lima Diniz Bas´ılio 0 1
C´ıcero Fla´vio Soares Araga˜o 0 1
Rui Oliveira Macedo 0 1
Fa´bio Santos de Souza 0 1
0 Programa de Po ́s-graduac ̧a ̃o em Cieˆncias Farmaceˆuticas, Universidade Federal do Rio Grande do Norte, Av. Gal. Gustavo C. de Farias , Natal, RN 59012-570 , Brazil
1 & Renata da Silva Leite
Thermoanalytical techniques have been applied in studies of herbal products. Myracrodruon urundeuva Allema˜o (Anacardiaceae) is a native of Brazil with medicinal properties. This study aimed to characterize the dry extracts of M. urundeuva Allema˜o and to assess the compatibility of extracts with pharmaceutical excipients in physical mixtures using thermogravimetry (TG) and differential thermal analysis (DTA). The TG curve of M. urundeuva dry extract (ES) showed the occurrence of four mass loss events. The most significant mass loss of extract was observed between 193.5 and 267.0 C with a loss of 29.7%. The DTA curve showed the endothermic nature of this event with a peak at 235.8 C (DH = 568.5 J g-1). This event is associated with the thermal decomposition of carbohydrates and other organic compounds present in the plant. The SEM image showed the particles of dry extract with spherical shapes, irregular sizes and rough surfaces. SEM analysis of physical mixtures showed that extract dry particles maintained their spherical morphology and appeared uniformly dispersed in the excipient particles. The TG and DTA curves showed no thermal incompatibility between the ES and the excipients lactose, cellulose
Myracrodruon urundeuva Allema˜o extract; TG; DTA; Spray dryer; SEM
Departamento de Cieˆncias Farmaceˆuticas, Universidade
Federal de Pernambuco, UFPE, Av. Prof. Moraes Rego, 1235
Cidade Universita´ria, Recife, PE 50670-901, Brazil
Laborato´rios Unificados de Desenvolvimento e Ensaios de
Medicamentos, LUDEM, Universidade Federal da Para´ıba,
UFPB, Campus I, Joa˜o Pessoa, PB 58059-900, Brazil
and starch, but indicated a possible interaction with
The Myracrodruon urundeuva Allema˜o is an arboreal
species of the Anacardiaceae family native to Brazil,
commonly known as ‘‘aroeira-do-serta˜o,’’
‘‘aroeira-docerrado’’ and ‘‘aroeira-preta’’ [
]. Studies have shown
], anti-inflammatory [
] and neuroprotective [
] properties, as well
as cytotoxicity in cancer cells .
The use of dry extracts in the production of herbal
medicines in the pharmaceutical industry has been
employed because of their advantages over liquid extracts
due to their greater stability (chemical, physical–chemical
and microbiological), higher concentrations of active
compounds, the ease of patterning and handling and a
greater processing capacity in different dosage forms
Among the techniques successfully employed in the
preparation of dry plant extracts, nebulization by spray
dryer is highlighted. This technique produces powders with
defined characteristics such as shape and particle size, and
rapid evaporation of the solvent reduces the process time
and risk of changes in thermolabile products such as plant
Thermal analysis has been widely used as a reliable
analytical tool in the physical and chemical investigation of
drugs in the control of quality and development of new
pharmaceutical formulations, in studies of stability and
compatibility, and in possible interactions between the drug
and excipients [
]. These techniques have also been
applied to the analysis of raw materials and plant products.
A study evaluated the thermal stability and kinetics of
degradation of extracts of Cissampelos sympodialis Eichi
using TG . Sampaio et al. [
] used TG and DTA to
characterize thermally dry extracts of Arrabidaea chica
obtained by spray drying. Medeiros et al. [
] evaluated the
presence of colloidal silicon dioxide and cyclodextrin
during the drying of extracts of Albizia inopinata using TG,
demonstrating the greater stability of the extracts with
cyclodextrin. Studies with TG were used to determine the
moisture and ash content of commercial samples of
Paullinia cupana Kunth in coffee powder in natura. The results
showed no difference between the data obtained by
conventional methods compared with the TG [
]. Costa et al.
], using DSC and TG, evaluated the degree of
compatibility of a lyophilized Heliotropium indicum extract
with hydroxyethylcellulose, methylparaben and propylene
glycol, showing that the latter two substances interacted
with the extract.
This study aimed to characterize the dry extracts of M.
urundeuva Allema˜o and to assess the compatibility of
extracts with pharmaceutical excipients in physical
mixtures using thermogravimetry (TG) and differential thermal
In the study, leaves of M. urundeuva Allema˜o collected at
Carau´bas in the state of Paraiba, Brazil, were used. A
voucher specimen of this species was recorded in Lauro
Pires Xavier Herbarium under the registration no. NC240,
and botanical identification was carried out by Professor
Alecksandra Vieira de Lacerda of the Federal University of
Campina Grande. The plant material was clean, oven-dried
at a temperature of 50 ± 2 C for 96 h, ground in a
mechanical mill and stored in sealed plastic bag until used.
The hydroethanolic extract of leaves (10 L) was obtained
by the maceration of 2 kg of powdered leaves in a solution
of 50:50 (v v-1) ethanol/water for 120 h.
flow rate of 62 m3 h-1 and a 2.0 bar of pressure. The
colloidal silicon dioxide (Henrifarma, Lot 3157052414,
Brazil) was used at 10% (mass/mass) as a drying agent.
Obtaining binary mixtures
In the study, the following pharmaceutical excipients were
used: lactose monohydrate 200 mesh (Pharma shows, Lot
3367, Brazil), cellulose microcrystalline PH 102
(Purifarma, Lot C1312098, Brazil), pregelatinized starch
(Henrifarma, Lot GDI0258 * 036 710/15, Brazil) and
maltodextrin DE 20 (Pharma Nostra Comerc, Lot 746158,
Brazil), identified as LAC, CEL, AMD and MALT,
respectively. Binary mixtures were prepared by the
physical mixing of the dry extract of M. urundeuva Allema˜o
(ES) with pharmaceutical excipient in the proportion of 1:1
The curves dynamic TG and DTA of nebulized extract,
pharmaceutical excipients and binary mixtures were
obtained using the same thermobalance model DTG-60
(Shimadzu, Kyoto, Japan) in a heating rate of 10 C min-1
from 25 to 800 C in an atmosphere of nitrogen with a
constant flow of 100 mL min-1. The samples were placed
in alumina crucible with a mass around 5.0 (± 0.5) mg.
The equipment was calibrated using TG calcium oxalate
monohydrate. The TG and DTA curves were analyzed by
the RT-60 W program (Shimadzu).
Scanning electron microscopy (SEM)
The morphology of shape and surface characteristics of M.
urundeuva dry extracts and binary mixtures was assessed
using scanning electron microscopy (Hitachi TM–1000,
Hiscope—New Jersey, USA) under an atmospheric
vacuum of 5–10 Torr. The images were captured with a
voltage acceleration of 15 kV. Samples were metallized by
spraying gold and were subsequently displayed in different
Results and discussion
The hydroethanolic extract of M. urundeuva Allema˜o was
subjected to the drying process in the spray dryer model
SD-05 (Lab-Plant, Huddersfield, UK). The drying
conditions were inlet air temperature in the dryer of 180 C and
a feed rate of 8 mL min-1. The atomizer double pneumatic
fluid nozzle with 1.2-mm opening hole operated with an air
The TG curve of M. urundeuva Allema˜o dry extract (ES)
showed the occurrence of four mass loss events (Fig. 1).
The first occurred in a temperature range of 41.8–103.1 C,
and the mass loss was 2.9%, probably corresponding to
dehydration and to a loss of volatile compounds present in
the sample. The DTA curve showed the endothermic nature
of this process with a peak at 69.0 C (DH = 262.6 J g-1).
The second event, with a mass loss of 5.0%, occurred in a
temperature range between 105.1 and 189.5 C,
corresponding to the first extract decomposition step. The most
significant mass loss of extract was observed between
193.5 and 267.0 C with a loss of 29.7%. The DTA curve
showed the endothermic nature of this event with a peak at
235.8 C (DH = 568.5 J g-1). This event is associated
with the thermal decomposition of carbohydrates and other
organic compounds present in the plant [
]. Studies of
phytochemicals identified the presence of carbohydrates,
tannins, flavonoids, monoterpenes and sesquiterpenes,
triterpenes and steroids, condensed proanthocyanidins and
] in the species under study.
The fourth step of mass loss was 13.5% and occurred
between 280.5 and 372.5 C, probably corresponding to a
degradation of more stable compounds and the beginning
of the formation of ashes [
]. A 48.9% residue was
observed, which can be attributed to the mass of the
colloidal silicon dioxide, which makes up 10% of the sample
added to the carboxylate residue and the ash content
corresponding to the minerals in the sample.
The TG and DTA curves of the dry extract of M.
urundeuva Allema˜o and physical mixtures are shown in
Lactose is composed of white crystalline particles used
as adjuvant pharmaceutics due to its binder and diluent
action in the production of tablets and capsules. The most
common commercially available lactose is a-lactose
monohydrate and b-lactose [
]. The DTA curve of lactose
(Fig. 2a, b) showed two endothermic peaks in range of
118–324 C. The first peak is related to a LAC dehydration
process that occurred at 148.6 C (DH = 1.1 kJ g-1) and
was also observed in the TG curve with a mass loss of 4.6%
(Tonset = 141.1 C; Tendset = 150.1 C) attributed to the
lactose monohydrate presenting 5% stoichiometric water
]. The second peak showed a fusion of LAC at 219.2 C
(DH = 566.4 J g-1); the thermal decomposition process of
the excipient then occurred, confirmed by the TG curve
with two steps of mass loss, 15.2% (Tonset = 236.5 C;
Tendset = 252.8 C) and 31.2% (Tonset = 302.6 C; Tendset
= 314.5 C) respectively. These peaks characterized
alactose monohydrate [
]. In temperature range
324–800 C, two endothermic peaks with a wide
temperature range and low reproducibility were observed
corresponding to the processes of lactose decomposition.
The thermal behavior of the physical mixture ES–LAC
was similar to the profiles of the samples of ES and LAC
individually (Fig. 2a, b). The DTA curve of the mixture
showed an endothermic event between 72.4 and 80.7 C
(DH = 45.5 J g-1) corresponding to a loss of water and
volatile components of the mixture as observed in ES and
also in LAC. An endothermic peak at 147.1 C
(DH = 45.5 J g-1) was observed in the TG curve with a
mass loss of 3.4% (Tonset = 136.2 C; Tendset = 148.2 C).
Another endothermic peak was observed at 210.1 C
(DH = 694.2 J g-1) in the TG curve corresponding to the
thermal decomposition step with a mass loss of 19.8%
(Tonset = 205.4 C; Tendset = 225.2 C). Thus, the ES–
LAC mixture had thermal events resulting in ES and LAC
individually, indicating that there was no apparent
incompatibility between the LAC and the ES.
The microcrystalline cellulose is supplied as a white
crystalline powder used in pharmaceutical solid
formulations as a diluent, binder, suspending agent, lubricant,
disintegrant and adsorbent [
]. The DTA curve of the
microcrystalline cellulose PH-102 (Fig. 2c, d) showed a
broad endothermic peak at 54.6 C (DH = 618.3 J g-1),
which corresponded to the removal of surface water of the
excipient, and an endothermic peak corresponding to the
thermal decomposition and depolymerization of the CEL at
343.4 C (DH = 3.99 kJ g-1). The TG curve showed a
loss of water of CEL with a mass loss of 2.8% (Tonset
= 34.0 C; Tendset = 64.0 C) and thermal decomposition
process of CEL in a single step with a mass loss of 87.6%
(Tonset = 324.8 C; Tendset = 355.3 C). The results were
similar to those reported in [
] the literature.
The DTA curve of the ES–CEL mixture showed three
endothermal events equivalent to the three steps of mass
loss in a TG curve (Fig. 2c, d). The first event occurred
between 40.2 and 95.1 C (DH = 327.5 J g-1), and the TG
curve showed mass loss of 2.3% (Tonset = 48.5 C; Tendset
= 79 C), corresponding to a loss of water and volatile
components ES (as noted in ES and also in the CEL). The
second peak occurred at 229.3 C (DH = 218.9 J g-1),
and the TG curve showed a mass loss of 16.6% (Tonset
= 207.7 C; Tendset = 235.6 C), corresponding to a
degradation of ES as noted. The third peak occurred at
360.5 C (DH = 1.1 kJ g-1), and the TG curve showed a
mass loss of 32.7% (Tonset = 339.1 C;
300 400 500
100 200 300 400 500 600 700 800
The DTA curve of AMD showed two endothermic peaks
(Fig. 2e, f). The first at 74.0 C (DH = 832 J g-1)
corresponded to dehydration and gelatinization of the excipient
with mass loss in a TG curve of 4.2% (Tonset = 52.2 C;
Tendset = 94.4 C) and the second at 320.1 C
(DH = 3.99 kJ g-1), corresponding to the elimination of
polyhydroxy groups accompanied by depolymerization and
decomposition of the starch in the TG curve with a mass
loss of 73.8% (Tonset = 301.7 C; Tendset = 329.2 C) [
There was no evidence of interaction of ES with AMD
since the TG and DTA curves of the mixture can be
regarded as a superposition of the curves individual of ES
and AMD. The DTA curve of the mixture showed an
endothermic peak at 72.2 C (DH = 409.6 J g-1),
attributed to the dehydration of the sample as occurred in ES
and AMD, and an endothermic peak at 226.5 C
(DH = 265.4 J g-1), corresponding to a degradation of ES.
An endothermic event was also observed between 327 C
and 271.6 (DH = 314.8 J g-1), corresponding to the
degradation of AMD.
The DTA curve of MALT excipient (Fig. 2g, h) showed
the first endothermic event between 43.9 and 147.6 C
(DH = 1.1 kJ g-1), and the TG curve showed a mass loss
of 4.6% (Tonset = 46.5 C and Tendset = 112.6 C),
corresponding to a loss of water and the glass transition carrier
]. The second event occurred between 225.3 and
275.1 C (DH = 482.4 J g-1), and the TG curve showed a
mass loss of 11.3% (Tonset = 247.2 C; Tendset =
278.6 C), corresponding to the dextrinization of the
33, 35, 36
]. The third endothermic event showed a
peak at 318.5 C (DH = 4.1 kJ g-1), and the TG curve
showed a mass loss of 37.5% (Tonset = 292.7 C; Tendset =
320.9 C), corresponding to the decomposition and
depolymerization of the MALT. An exothermic event was
observed between 506.9 and 519.1 C (DH = 3.3 kJ g-1),
which may be related to gaseous products such as carbon
dioxide and carbon monoxide resulting from the final
processes of degradation of MALT [
The DTA curve of the mixture ES–MALT (Fig. 2g, h)
showed that there were three endothermic events. The first
event occurred between 66.6 and 101.8 C
(DH = 269 J g-1) in the TG curve, corresponding to a
mass loss of 4.8% (Tonset = 65.2 C; Tendset = 95.1 C).
This event is related to a loss of volatiles, and dehydrating
the mixture was observed in the sample of ES and also in
excipient. The other endothermic events corresponded in
the TG curve to two steps of mass loss of mixture, the first
of 15.6% (Tonset = 202.4 C; Tendset = 224.6 C) and the
second of 36.3% (Tonset = 283.8 C; Tendset = 322.9 C),
corresponding to the overlapping of the degradation of ES
and MALT. The most intense endothermic and exothermic
peaks were observed in the DTA curve; a MALT sample
was not observed in the mixture, indicating a possible
interaction between ES and MALT.
Scanning electron microscopy (SEM)
The morphology of samples of M. urundeuva Allema˜o dry
extract was analyzed by SEM, and images are presented in
Fig. 3. It can be observed that particles showed spherical
shapes with irregular sizes and rough surfaces. These
characteristics are generally found in dry extracts of plants
obtained by spray dryer and influence the flow properties
and bulk density of the product and exhibit homogeneity
and better particle size distribution [
SEM analysis of physical mixtures showed that extract
dry particles maintained their spherical morphology and
appeared uniformly dispersed in the excipient particles of
lactose, amid, cellulose and maltodextrin (Fig. 4). This
indicated a low tendency of ES agglomeration with the
excipients studied, favoring the uniform distribution of ES
particles in the mixtures, which is important for the
technological quality of the product to be developed.
The thermal study of ES showed a defined thermal
behavior with four stages of mass loss with proper
reproducibility and can be applied in the characterization of
standardized dry extracts.
The TG and DTA curves showed no thermal
incompatibility between the ES and the excipients lactose,
cellulose and starch, but indicated a possible interaction with
maltodextrin. SEM images of dry extract showed spherical
shapes with irregular sizes and rough surfaces and, physical
mixtures showed that dry extract appeared uniformly
dispersed in the excipient particles studied. Thus, the
characterization of the dried extracts of M. urundeuva by
TG, DTA and SEM provided important data that can be
used as a quality control parameter and as a tool for the
selection of excipients in product preformulation studies
using this plant.
Acknowledgements The authors acknowledge the fellowships
received from Conselho Nacional de Pesquisa (CNPq).
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