Journal of Thermal Analysis and Calorimetry

https://doi.org/10.1007/s10973-019-08073-3(0123456789().,-volV)(0123456789().
,- volV)

Thermal characterization of Aspidosperma pyrifolium Mart. plant drugs

Jéssica Cabral Andrade1 • Widson Michael Santos1 • Fernanda Pontes Nóbrega1 • Lucas Ferreira Almeida1 •

Felipe Hugo Alencar Fernandes1,2 • Cleildo Pereira Santana3 • Germano Véras4 •

Ana Cláudia Dantas Medeiros1

Received: 31 August 2018 / Accepted: 2 February 2019

Ó Akadémiai Kiadó, Budapest, Hungary 2019

Abstract
Aspidosperma pyrifolium Mart. is an endemic plant from Brazilian northeastern, which is widely used in folk medicine to
treat dermatitis, gastritis, and malaria due to its anti-inflammatory activity. Thus, the aim of this work was to characterize
by analytical techniques A. pyrifolium in different particle sizes to use in the production of tea. For characterization,
thermal analysis, optical microscopy, and near-infrared spectroscopy (NIR) techniques were used. After sieving, five
samples, named AP01 ([ 355 lm), AP02 (C 180 lm), AP03 (C 155 lm), AP04 (C 75 lm), and AP05 (C 38 lm), were
obtained. Thermogravimetry curves showed three steps of decomposition, with different percentages of mass loss. The
second step of decomposition showed the highest mass loss for the five samples. DTA curves of five samples showed a first
endothermic peak at 91.70, 96.22, 96.29, 91.09, and 86.32 °C for AP01, AP02, AP03, AP04, and AP05, respectively.
Decomposition of all particles occurred from 200 °C. The activation energy obtained through kinetic models showed
significant differences between the two methodologies employed. NIR spectra were treated using chemometric tools,
including principal component analysis and two PC were necessary to properly separate the samples. The analytical
techniques used in this study allowed us to properly characterize the powders and could be used in the production of tea.

Keywords Quality control  Analytical techniques  Chemometrics  Pereiro  Tea

Introduction

The Brazilian Pharmacopoeia and its official codes estab-

& Ana Cláudia Dantas Medeiros
anaclaudia@uepb.edu.br
1
Laboratório de Desenvolvimento e Ensaios de
Medicamentos, Centro de Ciências Biológicas e da Saúde,
Universidade Estadual da Paraı́ba, R. Baraúnas, 351, Cidade
Universitária, Campina Grande, Paraı́ba 58429-500, Brazil
2 control of the granulometry is an important step, since the
Unifacisa, Centro Universitário, Av. Sen. Argemiro de
Figueiredo, 1901, Itararé, Campina Grande,
Paraı́ba 58411-020, Brazil
3
Centro de Tecnologia em Desenvolvimento de Medicamentos
(CT-Tecnologia Farmacêutica), Faculdade de Farmácia,
Universidade Federal de Minas Gerais, Av. Pres. Antônio
Carlos, 6627, Belo Horizonte, Minas Gerais 31270-901,
Brazil
4
Laboratório de Quı́mica Analı́tica e Quimiometria, Centro de
Ciências e Tecnologia, Universidade Estadual da Paraı́ba, R.
Baraúnas, 351, Cidade Universitária, Campina Grande,
Paraı́ba 58429-500, Brazil
lish parameters to evaluate the quality of pharmaceutical
ingredients. However, for active vegetal pharmaceutical
ingredients, these parameters are scarce for several plant
species. Obtaining a herbal medicine requires safeguarding
the pharmacological and chemical qualities of the plant to
ensure that the biological activity and safety of the medi-
cation are not affected. During the production process, the
different sizes of the particles directly influence the char-
acteristics of the final product. Consequently, analytical
methods used are useful to characterize plant drugs,
ensuring the efficacy and efficiency of its usage by com-
panies during the production and quality control stages
[1, 2].
The International Confederation of Thermal Analysis
and Calorimetry (ICTAC) establishes that parameters for
non-isothermal kinetics studies should be determined
through free models, i.e., isoconversional models, which

123

are divided into two categories: differential and integral.
Many isoconversion mathematical models have been used
to characterize active pharmaceutical ingredients, such as
Flynn–Wall–Ozawa (FWO), Kissinger–Akira–Sunose
(KAS), Friedman, Li-Tang, modified Coats-Redfern, and
Vyazovkin [3]. Using methodologies obtained from ther-
mal studies, it is possible to obtain more precise informa-
tion to determine thermally stable raw materials [4].
Compared to other analytical techniques, optical
microscopy, although simple, is a useful tool that provides
images of the morphology of particles. This technique, for
example, was used in a preformulation study using
Schinopsis brasiliensis Engler and pharmaceutical excipi-
ents to identify incompatibilities [5].
The near-infrared (NIR) is a vibrational spectroscopy
technique that permits rapid analysis without chemical
reactions [6] in samples of beverages, cigarettes, food, fuel,
and drugs. However, this analytical technique presents very
complex spectral signals; therefore, chemometrics, specif-
ically multivariate analysis, are necessary to treat the data.
Thus, it is possible to concentrate the analytes or chemical,
physical, or physical–chemical properties in a chemometric
technique called multivariate calibration. However, it is
also possible to cluster the samples, resulting in pattern
recognition. The most used technique to cluster samples is
principal component analysis (PCA), which is used in the
analysis of particle size [7].
The Apocynaceae family presents a great morphological
variety, characterized by the presence of lactic vessels and
a diversity of secondary metabolites such as cardiac gly-
cosides and indolic alkaloids, which are involved in phar-
macological activities. The genus Aspidosperma presents a
major phytochemical relevance and is mostly found in
South America, in biomes such as Cerrado and Caatinga,
and in some forests. A. pyrifolium is a relevant species in
folk medicine. Commonly known as ‘‘Pereiro’’, it is used to
treat various conditions such as dermatitis, gastritis, and
malaria due to its anti-inflammatory activity [8, 9].
The production of particles is a critical step because any
change in their granulation can result in particles with
heterogeneous and non-uniform sizes. Therefore, the ana-
lytical methods used are useful for characterizing plant
drug materials, ensuring the efficacy and effectivity of their
use by companies during the production and quality control
stages of tea [10, 11].
Thus, the aim of this work was to characterize by ana-
lytical techniques Aspidosperma pyrifolium Mart. in dif-
ferent particle sizes to use in the production of tea.
123
J. C. Andrade et al.
Materials and methods
Powder obtention
The bark of A. pyrifolium was collected in the semiarid
region of Paraı́ba, Brazil (7°130 5000 S, 520 5200 W). The vou-
cher specimen was prepared and identified at the Professor
Leonardo Pessoa Felix Herbarium, Federal University of
Paraı́ba, under number 20104.
The plant material was oven-dried at 40 °C and pul-
verized on a knife mill, with a 10-mesh screen coupled.
The plant drugs were submitted to sieves of different mesh
([ 355, C 180, C 150, C 75, and C 38 lm). The powders
obtained, with different granulometry, were named AP01
([ 355), AP02 (C 180), AP03 (C 150), AP04 (C 75), and
AP05 (C 38 lm) and separately packed in properly closed
polyethylene bottles, protected from light and moisture and
stored at room temperature, at 25 °C.
Differential thermal analysis (DTA)
Differential thermal analysis (DTA) curves of the powders
(AP01, AP02, AP03, AP04, AP05) were obtained in a
Shimadzu (DTG-60) thermal analyzer using aluminum
crucibles with 2 ± 0.1 mg samples, under nitrogen atmo-
sphere at 50 mL min-1 flow rate. The experiments were
carried out in the temperature range of 25–450 °C, with a
heating rate of 10 °C min-1.
Thermogravimetry (TG)
The dynamic thermogravimetric curves of the powders
(AP01, AP02, AP03, AP04, AP05) were obtained in a
Shimadzu (DTG-60) thermal analyzer using alumina cru-
cibles with 8 ± 0.1 mg samples, under nitrogen atmo-
sphere at a 50 mL min-1 flow rate. The experiments were
carried out in the temperature range of 25–900 °C, with a
heating rate of 10 °C min-1.
Kinetic study of particles
Thermogravimetric analyses were performed in a simulta-
neous thermal analyzer (Shimadzu DTG-60). Samples
(8 ± 0.1 mg) were analyzed in alumina pans, under
nitrogen atmosphere with a flow of 50 mL min-1, heating
rates of 10, 20 and 40 °C min-1, and a temperature range
from 25 to 900 °C. The FWO and KAS were used to
determine the parameters of thermal analysis kinetics.
Thermal characterization of Aspidosperma pyrifolium Mart. plant drugs

The FWO equation is written as Results and discussion

 
0:0048AE E
ln b ¼ ln  1:0516 ð1Þ Differential thermal analysis (DTA)
RGðaÞ RT
The KAS equation is written as The DTA curves of the herbal drug powders in the different
   
b AR E particle sizes (Fig. 1) show events due to phase transitions
ln 2
¼ ln  ð2Þ as a function of the temperature. In these occurrences,
T EGðaÞ RT
thermal events are evidenced that are characteristic of the
where b is the linear heating rate (°C min-1); E is the decomposition of the plant drugs.
activation energy (J mol-1); A is the pre-exponential fac- The first endothermic peaks in the curves of the five
tor; R is the molar gas constant; and G(a) is the integral samples represent peak temperatures between 91.70 and
mechanism function [12]. 86.32 °C for AP01, AP02, AP03, AP04, and AP05,
respectively, with initial temperatures between 35.78 and
Optical microscopy 50.54 °C. One of the characteristics of herbal drugs is to
present amorphous morphology, and thus, endothermic
Physical parameters such as circumference radius, diame- events can be attributed to the evaporation of water from
ter, and area of powder particles were evaluated by video room humidity once the amorphous matrices are too
microscopy using a HiroxÒ digital optical microscope, hygroscopic. The degradation processes of the particles
model KH 770. These measurements were determined by started at 200 °C. These processes occur due to the thermal
the average of 20 measurements. decomposition of certain secondary metabolites, such as
flavonoids, polyphenols, saponins [13], and alkaloids [14].
Near-infrared spectroscopy (NIR) The second endothermic event for all particles occurred
in the range of 137.99–200.80 °C, with peak temperatures
Absorption spectra in the near-infrared region were between 183.35 and 185.84 °C.
obtained with a PerkinElmerÒ Lambda 750 spectropho- The third exothermic event occurred in the temperature
tometer in the region of 750–2500 nm, with resolution of range between 322.36 and 382.68 °C, with peak tempera-
2 nm, using Praying MantisÒ accessory, in reflectance tures between 383.00 and 349.11 °C, respectively, for
mode. The powders of the plant drugs were analyzed AP01, AP02, AP03, AP04, and AP05 (Table 1). Variations
quintuplicate (n = 5) and the spectral curve constructed, of Tonset, Tendset, and enthalpy of the three thermal events
from the average of the five curves obtained. The NIR observed in DTA curves are suggestive of differences in
spectra were used to characterize the powders and verify the thermal behavior of particles. The enthalpy reduction
differences in size between the samples and clustering. observed in the second endothermic event for the AP05

Chemometric analysis AP01

AP02
Spectroscopic data, from the powders with different par- 0 AP03
AP04
Temperature difference/µV ; Exo up

ticle sizes, were submitted to unsupervised pattern recog- AP05

nition principal component analysis, using the software the
Unscrambler 9.8. For better visualization of the data, they –3
were preprocessed, where a baseline correction of the
spectra was performed.
–6

Statistical analysis

Data were analyzed using BioStat statistical software, –9

version 5.3. Results were expressed as mean ± SEM.
Comparisons between groups were made using nonpara-
– 12
metric ANOVA (Kruskal–Wallis) followed by post hoc
50 100 150 200 250 300 350 400 450 500
Dunn’s multiple comparison test. At 95% confidence
Temperature/°C
interval (p \ 0.05), the difference between the compared
groups was considered as statistically significant. Fig. 1 DTA curves of the particles: AP01, AP02, AP03, AP04, and
AP05

123
 J. C. Andrade et al.

Table 1 Data of the differential thermal analysis of the particles

Samples Peak 1 Peak 2 Peak 3
-1 -1
Tpeak/°C DH/J g Tonset and endset/°C Tpeak/°C DH/J g Tonset and endset/°C Tpeak/°C DH/J g-1 Tonset and endset/°C

AP01 91.70 242.93 63.07–117.43 183.53 94.25 161.91–200.80 383.00 154.40 373.90–437.53
AP02 96.22 260.42 66.12–124.46 185.84 56.08 159.15–198.45 382.68 106.95 335.76–382.68
AP03 96.29 501.02 35.78–130.53 183.35 47.35 157.85–196.58 341.43 17.42 324.22–360.63
AP04 91.09 360.75 111.15–115.80 136.54 28.96 148.57–189.53 327.37 35.31 323.87–353.36
AP05 86.32 322.19 51.59–112.38 179.83 96.92 137.99–189.13 349.11 1.07 322.36–433.11

particle may be associated with the presence of macro- Thermogravimetry (TG)

components, such as cellulose and lignins; these elements
maintain the basic needs of the plant and may occur in
quantities with larger particle sizes of a higher energy
release to degrade these components.
Differential thermal analysis is based on the interpreta-
tion of endothermic and exothermic events, which appear
along the DTA curves. These events provide, for example,
qualitative and quantitative physicochemical information
from the format and position of such peaks [15].
Plant materials are composed of complex matrices. This
impairs the quality of peaks in DTA, where the poor
quality of peaks can be attributed to some factors, such as
imperfections of the particles that constitute the plant
drugs, loss of gaseous products in the heating of the sam-
ple, and presence of impurities. These factors contribute to
endothermic peaks with defective widths [16, 17]. In
Table 2, the DTA data are listed.
Table 2 Data of initial decomposition temperature of the particles
Samples Tonset/°C Tendset/°C
The thermogravimetric curves of the plant drug powders
presented three stages of decomposition. The first stage
(Fig. 2) occurred at a temperature range from 19.77 to
78.50 °C, which can be attributed to the loss of volatile
compounds and probably residual water in the samples. For
this stage, the mass losses were 9.98, 7.76, 8.35, 7.70, and
5.96% for AP01, AP02, AP03, AP04, and AP05,
respectively.
To perform the quality control of active pharmaceutical
vegetal ingredients, the Brazilian Pharmacopoeia estab-
lishes a maximum limit of 14% for humidity. The TG
results make it possible to determine the moisture content
of the plant drugs and, with these results, establish manners
to control drying parameters, thus avoiding the growth of
microorganisms, chemical reactions, and the subsequent
degradation of the samples [2].
Larger molecules are degraded in the following steps, as
can be attributed to the second event. This event occurred
in the range of 259.06 to 363.68 °C with a mass loss of
Mass loss/%

AP01 63.76 76.70 9.98 100

280.00 349.29 54.64 AP01
AP02
498.56 606.20 23.94 80 AP03
AP02 55.58 78.50 7.76 AP04
60 AP05
Mass/%

279.82 363.68 56.57

508.34 610.65 10.15
40
AP03 52.01 67.36 8.35
269.33 362.74 55.20
20
675.94 904.80 12.78
AP04 51.47 71.49 7.70 0
259.06 353.13 53.95
431.11 562.43 13.55 0 100 200 300 400 500 600 700 800 900
AP05 19.77 65.01 5.96 Temperature/°C
259.85 345.31 53.23
Fig. 2 TG curves of the particles: AP01, AP02, AP03, AP04, and
696.26 792.76 15.68
AP05

123
Thermal characterization of Aspidosperma pyrifolium Mart. plant drugs
54.64% for AP01, 56.57% for AP02, 55.20% for AP03,
53.95% for AP04, and 53.23% for AP05, representing the
stage with the highest degradation of samples. This step of
degradation occurred close to the temperature range of the
second thermal event of DTA curves.
The third step, with a start temperature of 431.11 °C and
a final temperature at 904.80 °C, presented a mass loss of
23.94, 10.15, 12.78, 13.55, and 15.68% for AP01, AP02,
AP03, AP04, and AP05, respectively, corresponding to the
ash content of the samples. In this step, the sample con-
stituents that were carbonized still have inorganic matter
and residues that may not degrade in such an atmosphere.
As the particle size decreases, the initial decomposition
temperature also decreases, indicating a possible difference
in the constitution of the molecules present in the plant
drug with different granulometry.
Vegetal matrices are composed of several components,
being a mixture of organic and inorganic compounds
[17, 18]. The thermal decomposition of these substances
are the results of physicochemical phenomena, which occur
after heating. Table 2 lists the values associated with the
thermogravimetric decomposition steps of the five samples
of A. pyrifolium.
Study of the kinetic behavior of the particles
The TG curves of the particles obtained in the heating rates
(b) of 10, 20, and 40 °C min-1 (Fig. 3) showed the same
thermal profile, with only a shift of curves due to the dif-
ferent heating rates. Heating rates may shift thermogravi-
metric events to higher or lower temperatures as well as
influence the number of decomposition steps, causing
variations in the mass loss values and thus inducing errors.
In this context, it is fundamental to use different heating
rates in thermogravimetric analysis [19, 20].
Activation energy represents a barrier through which
every chemical reaction needs to be transposed in order to
begin. It is one of the most important kinetic parameters to
be determined. The kinetic models used in the study were
Flynn–Wall–Ozawa and Kissinger–Akira–Sunose. The
temperature ranges and the mass loss (Table 3) obtained in
three heating rates of the second step of decomposition of
particles were selected, just after the decomposition step of
the volatile substances.
The kinetic models of Flynn–Wall–Ozawa (FWO) and
Kissinger–Akira–Sunose were applied using nine decom-
position fractions (0.1 \ a \ 0.9). The activation energy
(Ea) was calculated by the angular coefficient of the
straight lines obtained from the logarithm of b versus
1000 T-1 for the FWO model.
The activation energy (kJ mol-1) for the five particles
was calculated by multiplying the angular coefficient of the
line by the gas constant (R = 8.31 kJ mol-1). It was pos-
sible to observe that, in the FWO kinetic model (Table 3),
the mean activation energy of the particles was higher than
100 kJ mol-1, with a decrease for the particles AP04
(105.65 kJ mol-1) and AP05 (100.92 kJ mol-1).
For the kinetic study of KAS (Table 3), the mean acti-
vation energy of five particles increased as the diameter of
the particles decreased, but in the AP05, the mean activa-
tion energy decreased to 100.04 kJ mol-1, which is the
same value as that obtained from the Ozawa kinetic study.
These differences observed in our study may be related to
the occurrence of multiple events happening in the chosen
work range [21]. The powders with a larger surface area
showed to be more thermally unstable, requiring a lower
activation energy for thermal decomposition to occur. The
same results were found in the study by Brandão [1].
The analysis of variance and post hoc Tukey test indicated
that the FWO model was more sensitive than KAS for the
differentiation of the particle sizes in relation to its activation
energy. This can be explained because the KAS model takes
into account the peak temperature of the fractions (a) in the
construction of the kinetic mathematical model.
The influence of particle size on the mean activation
energy of the FWO method shows that the particles with a
smaller surface area have a higher resistance in the heat
transfer. This effect is more accentuated for the particles
AP01, AP02, and AP03, where this parameter can be taken
into account in the choice of the particle that will be used
as raw material in the manufacture of a phytotherapeutic
future. The KAS method also showed a decrease in the
activation energy due to the decrease in the particle size of
A. pyrifolium plant drugs.
123
 J. C. Andrade et al.

(a) 10 °C min–1 (b) 10 °C min–1

20 °C min–1 20 °C min–1
100 40 °C min–1 100 40 °C min–1

80 80
Mass/%

60 60

Mass/%
40 40

20 20

0 0

0 100 200 300 400 500 600 700 800 900 0 100 200 300 400 500 600 700 800 900
Temperature/°C Temperature/°C

(c) 10 °C min–1 (d) 10 °C min–1

20 °C min–1
20° C min–1
100 40 °C min–1 100 40 °C min–1

80 80
Mass/%
Mass/%

60
60

40
40

20
20
0
0
0 100 200 300 400 500 600 700 800 900 0 100 200 300 400 500 600 700 800 900
Temperature/°C Temperature/°C

(e) 10 °C min–1
20 °C min–1
100
40 °C min–1

80
Mass/%

60

40

20

0 100 200 300 400 500 600 700 800 900

Temperature/°C

Fig. 3 TG of the particles in different heating ratios: a AP01, b AP02, c AP03, d AP04, and e AP05

123
Thermal characterization of Aspidosperma pyrifolium Mart. plant drugs

Table 3 Activation energy

Samples Temperature zone (Tonset and enset/°C) Activation energies/kJ mol-1
obtained by the FWO and KAS
technique at predetermined (b) 10 °C min-1 (b) 20 °C min-1 (b) 40 °C min-1 FWO KAS
temperature intervals and in
different heating ratios AP01 265.74–300.80 243.43–280.09 222.22–255.23 100.92 ± 10.7 100.40 ± 11.8
AP02 224.72–251.04 243.03–271.56 250.03–272.56 117.76 ± 5.9 114.8 ± 5.1
AP03 225.35–321.57 259.54–277.32 252.65–273.25 118.85 ± 8.7 114.8 ± 14. 7
AP04 224.16–274.33 247.65–257.43 245.35–270.73 105.65 ± 15.2 115.98 ± 7.7
AP05 221.65–251.85 229.08–242.07 251.43–284.56 100. 92 ± 10.7 100.4 ± 11.7

(a) 500 µ m (b) 500 µ m

(c) 500 µ m (d) 500 µ m

(e) 500 µ m

Fig. 4 Optical microscopy of the plant drug in different particle sizes: 355 lm (a), 180 lm (b), 150 lm (c), 75 lm (d), and 38 lm (e)

123

Optical microscopy
The characterization of plant drugs is a step that allows a
better control in the development of a quality herbal
medicine. The standardization of powder granulometry of
herbal species should be considered, aiming at a strict
quality control [19]. Spherical particles have different
behaviors from those with a shape that does not fit in any of
the geometric forms, which requires an effective stan-
dardization since the particle shape serves as an indicator
of the reproducibility of a process [22].
Optical microscopy is a useful tool to verify particle sizes
and their distribution (Fig. 4). Using this technique, it was
possible to observe the morphological non-uniformity of
granules AP01 (Fig. 4a), AP02 (Fig. 4b), AP03 (Fig. 4c),
AP04 (Fig. 4d), and AP05 (Fig. 4e), which can be explained
by the efficiency of the pulverization process employed.
The mean diameter values obtained by microscopic
analysis were 258.0, 180.6, 173.2, 83.2, and 37.4 lm for
AP01, AP02, AP03, AP04, and AP05, respectively. The
AP03 and AP04 samples showed particles with higher
diameters than those specified on the sieves used in the
separation process.
Some factors may negatively favor the passage or
retention of the powder in the wrong mesh. Holes in the
mesh of the tamis facilitate the passage of larger particles,
and the moisture absorption by the powders can cause the
formation of granules, preventing the passage of smaller
particles or even their adhesion to specific places of the
sieves. Uneven agitation will also negatively influence the
separation process.
The particles can pass through the mesh in a number of
ways. As they do not have characteristic formats, the same
particle can pass through the sieve in the longitudinal
direction and thus not be classified correctly according to
its diameter. Furthermore, this same particle in the trans-
verse direction can be retained in a sieve that does not
correspond to its real diameter [19].
Near-infrared spectroscopy
To perform chemometric analysis, data were arranged in
matrices in which the lines (n) referred to the spectra of
samples and (i) referred to the variables analyzed in the
study. In the case of NIR spectral data, these refer to the
signals of reflectance transformed into absorbance.
The data matrix obtained after analysis consisted of 60
lines (samples) and 1404 columns (variables). The
obtained spectra were preprocessed in the data to high-
light the differences between samples. The most appro-
priate preprocessing technique, through which a better
visualization of the separation of the particles was
123
J. C. Andrade et al.
obtained, was baseline correction. This technique trans-
forms a sloping baseline into a horizontal baseline. By
performing preprocessing of the samples, the less
important information is eliminated, making the data
matrix clearer and thus allowing a subsequent exploratory
analysis of the data.
In the principal component analysis, three PCs were
selected, among which the first was capable of explain-
ing 94% of the data, and the second and third PCs
corresponded to 3% of the rest of the data. After the
third PC, the explained variance shows a slight decrease
(Fig. 5).
Samples are visualized on the score chart (Fig. 6), where
they are projected onto a new axis (PCs). According to the
granulometry of the powders, it was possible to visualize a
tendency and formation of groups, although there were
some similarities between some sizes obtained in the sep-
aration process.
The samples are visualized on the dot chart (Fig. 6),
where they are projected onto a new axis (PCs). After
visualizing the samples in the graph, it can be seen that
the samples form groups in accordance with the different
granulometry. This demonstrates that, although spectral
data are obtained from visually similar samples, the par-
ticles contain peculiarities that allow them to be distin-
guished from each other. The blue, green, red, black, and
yellow circles, distributed along the PC1 and PC2 axes,
correspond to samples AP01, AP02, AP03, AP04, and
AP05, respectively. The two samples that distance
themselves from the others (AP02) in the graph are
considered anomalous samples. These variables do not
influence exploratory data analysis. The differentiation of
the five particles with different granulometry, by the
chemical model, affirms the existence of the differences
between the particles with respect to their chemical con-
stitution, which was observed in the results from the use
of thermal methodologies.
The control of granulometry in the pharmaceutical industry
is a critical step in the development of herbal medicines. The
0.0030
0.0025
0.0020
0.0015
0.0010
PC1 PC2 PC3
0.0005
0
PC_00 PC_01 PC_02 PC_03 PC_04 PC_05
Fig. 5 Variance explained
Thermal characterization of Aspidosperma pyrifolium Mart. plant drugs
Fig. 6 Graphic of scores 2.0 PC2
1.5
1.0
0.5
– 0.5
– 1.0
–2 –1
Granulometry, X-expl 94%, 3%
state of partition of the plant drug will influence the extract
content of secondary metabolites and potentiate the pharma-
cological and toxicological effects [22]. Thus, there is a need to
implement a methodology to identify the degree of partitioning
of plant raw materials more quickly and efficiently.
Techniques that use chemical data of certain substances
can optimize the efficiency of granulometry control anal-
yses in the pharmaceutical industry. The implementation of
infrared spectroscopy is a widespread technique that gen-
erates fast results with a low consumption of samples.
Chemometric techniques applied to spectral data from NIR
can be used to improve the quality control of plant active
pharmaceutical ingredients, where there would be a more
efficient standardization of particle size [21, 22].
Conclusions
The thermoanalytical techniques provided initial and final
temperatures of the thermal events of the DTA, as well as
the energy involved in the process, which showed signifi-
cant differences for the five particles. The kinetic model of
FWO was more sensitive to detect differences in activation
energy between particles. Using optical microscopy, it was
concluded that the techniques used in the processing of
vegetal material to obtain particles of different sizes were
inefficient, evidencing the need to use fast, efficient tech-
niques, such as the use of spectroscopic data obtained in
the NIR, processed through chemometric tools.
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AP04
AP03
AP02
AP01
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