Brazilian Dental Journal (2014) 25(2): 153-159
http://dx.doi.org/10.1590/0103-6440201302209
ISSN 0103-6440
Characterization of Dentifrices
Containing Desensitizing
Agents, Triclosan or Whitening
Agents: EDX and SEM Analysis
Shelon Cristina Souza Pinto1, Sérgio Paulo Hilgenberg1, Denise Stadler
Wambier1, Paulo Vitor Farago1, Matheus Coelho Bandéca2, Fábio André
Santos1
Dentifrices with different compositions are available on the market, but there is limited
information about their properties. The aim of this in vitro study was to evaluate the
physicochemical characteristics of 12 dentifrices divided into three categories, as containing
desensitizing agents, Triclosan or whitening agents. Desiccation loss/residue analysis:
5 g of dentifrice was weighed five times for each group. pH analysis: 5 g of dentifrice
were diluted in three parts of distilled water and analyzed using a digital potentiometer.
Scanning electron microscopy (SEM): analysis of ashes, shape and size of the particles.
Energy-dispersive x-ray spectroscopy (EDX): identification of the abrasive elements. Data
were analyzed using ANOVA, Bonferroni post hoc test (α=0.05). Desiccation loss: 38.21%
to 65.83%. Dentifrices containing Triclosan and desensitizing agents showed statistically
significant differences among them (p<0.05). Whitening dentifrices showed statistically
significant differences between Close-Up Whitening and Sensodyne Branqueador (44.72%,
65.83%, respectively). Most dentifrices presented neutral or basic pH. Different shape and
size particles were observed in the SEM analysis. Abrasive elements were identified in the
EDX. These results demonstrate that the evaluated dentifrices had different properties
and their composition influences directly their characteristics, thus resulting in a more
or less abrasive action on tooth surface. Knowing the characteristics of the dentifrices
is important to indicate the ideal product for each case.
Introduction
The decrease in the prevalence of caries disease
is certainly due to the use of fluoride by most of the
population worldwide. Dentifrices are the greatest source
of fluorides. These agents are regularly used and the
formulation of dentifrices has been improved to enhance
their therapeutic properties by incorporating agents such
as triclosan, potassium nitrate, strontium chloride and
different abrasive substances (1,2).
In order to ensure their effectiveness, dentifrices
must have ideal physicochemical characteristics. To
remove supragingival biofilm, toothbrushing causes
disarrangement in the intermicrobial matrix. To remove
the pigmentation from the enamel surface, dentifrice
composition requires abrasives (2).
The abrasiveness control of dentifrices is an important
factor to be considered because dental staining varies
among the population and the continuous use of dentifrices
may cause problems like abrasion of tooth structure and
gingival recession (1,3). The use of dentifrices with high
concentration of abrasive agents after the consumption of
acid beverages may increase enamel and dentine abrasion
(4). Different abrasive agents, detergents or a combination
1Department
of Dentistry, School of
Dentistry, UEPG - Ponta Grossa State
University, Ponta Grossa, PR, Brazil
2Department of PostGraduation, School of Dentistry,
UniCEUMA - CEUMA University,
São Luis, MA, Brazil
Correspondence: Profa. Dra. Shelon
Cristina Souza Pinto, Avenida
General Carlos Cavalcanti, 4748,
84030-900 Ponta Grossa, PR,
Brasil. Tel: +55-42-9924-4198.
e-mail: shelonsouzap@gmail.com
Key Words: dentifrices,
triclosan, pH.
of formulations produce different sources of abrasion (5).
According to Worschech (6), the roughness of the dental
enamel may be increased by the continuous use of abrasive
dentifrices during at home bleaching therapy.
The ideal dentifrice promotes the cleaning of the dental
surface with minimum abrasion, without causing irritating
effects on oral mucosa (7). As shown by Kielbassa (8), in
addition to its abrasive potential, the acidity of dentifrice
may increase significantly enamel and dentin erosion.
Therefore, it is also necessary to know the pH of dentifrices
in order to know their abrasive potential and acidity.
The goal of this study was to evaluate physicochemical
characteristics of 12 dentifrices divided into three
categories: desensitizing dentifrices, triclosan-containing
dentifrices and whitening dentifrices. The null hypothesis
is that the tested dentifrices present no differences in the
evaluated characteristics.
Material and Methods
Considering their physicochemical characteristics and
differences in the properties, 12 dentifrices of different
brands, belonging to one of the following categories
were used: desensitizing dentifrices, triclosan-containing
Braz Dent J 25(2) 2014
dentifrices and whitening (Table 1).
The dentifrices were submitted to the tests of
desiccation loss and residue analysis; analysis of abrasive
agents by scanning electron microscopy (SEM); energydispersive x-ray spectroscopy (EDX); granulometry; and
pH analysis. For such purpose, 5 samples were used for
each dentifrice.
Desiccation Loss and Residue Analysis
The dentifrice was weighed on a Petri dish (5.0 g). This
procedure was repeated five times for each group. After
being weighed, the samples were heated in an oven at 105
ºC for 24 h. They were then weighed again, repeating this
process until the same weight was recorded in consecutive
checks. Loss by desiccation was calculated from the
difference between the initial and final weights.
pH Analysis
S.C.S. Pinto et al.
The pH was measured using a previously calibrated
digital potentiometer (DMPH-2; Digimed, São Paulo, SP,
Brazil). Measurements were performed only once for each
one of the five samples at a dilution of 5.0 g suspended in
three parts of distilled water (15 mL).
SEM and EDX Analyses
After desiccation, the dentifrices were placed in
porcelain crucibles and heated in a furnace at 650 °C to
produce ashes, which were analyzed with a SEM microscope
(Shimadzu SSX 550; Shimadzu do Brasil, São Paulo, SP,
Brazil), operated at 15 kV and 1000× magnification. EDX
microanalysis (Shimadzu SSX 550; Shimadzu do Brasil) was
performed to determine the presence of particular chemical
elements in the dentifrices. The spectrum was obtained at 15
Kv, with a spot size of 5 nm and a counting time of 300 s.
Statistical Analysis
The data were analyzed by one-way ANOVA with
Bonferroni post hoc test (α=0.05). All data were analyzed
with PASW Statistics (version 18; SPSS Inc., Chicago, IL,
USA).
Results
Desiccation Loss and Residue Analysis
Dentifrices Containing Desensitizing Agents: there
were statistically significant differences (p<0.05), except
between Sensodyne Original (SO) and Sensodyne Cool Gel.
For this group, Sensodyne Original and Sensodyne Cool
Gel showed larger amount of solid residues (64.07% and
60.85%, respectively, Table 2).
Triclosan-Containing Dentifrices: there were statistically
significant differences (p<0.05), except between Sensodyne
Total Protection and Close-Up Gel. For this group, Prevent
and Sensodyne Total Protection have shown larger amount
of solid residues (55.16% and 40.92%, respectively, Table 2).
Dentifrices Containing Whitening Agents: there were
statistically significant differences between Close-Up
Whitening and Sensodyne Branqueador (44.72% and
65.83%, respectively); Sorriso Branqueador and Sensodyne
Branqueador (39.90% and 65.83%, respectively); Sensodyne
Branqueador and Colgate Sensitive Branqueador (65.83%
Table 1. Main agents presents in composition of the dentifrices evaluated
Groups
Dentifrices
containing
desensitizing
agents
Triclosancontaining
dentifrices
Dentifrices
containing
whitening agents
154
Trademark
Manufacturer
Fluoride
(ppm)
Colgate Sensitive
Colgate-Palmolive
Sensodyne Original
GlaxoSmithKline
Sensodyne Bicarbonato de Sódio
GlaxoSmithKline
Sensodyne – Cool Gel
GlaxoSmithKline
1100
Colgate Total 12
Colgate-Palmolive
1450
+
Sensodyne Proteção Total
GlaxoSmithKline
1400
+
Close-Up Gel
Unilever
1500
+
Prevent Anti-Placa
Colgate-Palmolive
Close-Up Whitening
Unilever
1500
Perlite
-
Sorriso Branqueador
Colgate-Palmolive
1500
Alumina
-
Sensodyne Branqueador
GlaxoSmithKline
1500
Amorphous silica
-
Colgate Sensitive Branqueador
Colgate-Palmolive
1450
Hidrous silica
-
Bleaching agent
Desensitizing agent
Triclosan
1500
5% potassium citrate
-
1490
10% strontium chloride
-
5% potassium nitrate
-
5% potassium nitrate
-
+
Braz Dent J 25(2) 2014
pH Analysis
Dentifrices pH are shown in Table 3. There were
statistically significant differences (p<0.05) among groups
(Table 3). Most dentifrices presented neutral or basic
pH, except Prevent Anti-Placa and Sensodyne Cool Gel
dentifrices (Group 1 - 6.37 ± 0.046 and Group 2 - pH 6.33
± 0.066, respectively).
SEM and EDX Analyses
Dentifrices Containing Desensitizing Agents (Fig. 1)
Colgate Sensitive: SEM micrographs showed spherical
and rounded particles. Some particles were joined and
arranged in conglomerates, but not sharp. Particle shape
showed less abrasive characteristics.
Sensodyne Bicarbonato de Sódio [Sodium Bicarbonate]:
Several clusters of small spherical particles could be
observed. Some SEM micrographs revealed particles that
Table 2. Results for desiccation loss and residue analysis of the dentifrices
Groups and dentifrices
Mean percent values
Dentifrices containing desensitizing agents
seemed to be dentifrice chips, which may have occurred
because the dentifrice in these samples was not entirely
in the ash form.
Sensodyne Cool Gel: It presented some small and
spherical particles and some large rhomboid and pointed
particles, which may indicate signs of greater abrasiveness.
Sensodyne Original: Smaller and spherical particles,
which may represent a minor abrasion.
Triclosan-Containing Dentifrices (Fig. 2)
Sensodyne Total Protection: SEM micrographs did not
show any particles.
Close Up Gel: Large and irregular particles, which may
indicate signs of greater abrasiveness.
Colgate Total 12: Small, rounded and irregular particles,
which may indicate some abrasiveness.
Prevent Antiplaque: Small, spherical and regular
particles, which may indicate little abrasiveness.
Dentifrices Containing Whitening Agents (Fig. 3)
Close Up Whitening: Large and irregular particles, which
may indicate greater abrasiveness.
Colgate Sensitive Whitening: Small and medium-sized
Table 3. Results for pH of the dentifrices
Dentifrices
Mean ± standard deviation
Dentifrices containing desensitizing agents
Colgate Sensitive
41.82% A
Colgate Sensitive
7.21 ± 0.013 A
Sensodyne Original
64.07% B
Sensodyne Original
7.81 ± 0.011 D
Sensodyne Bicarbonato de Sódio
51.40% C
Sensodyne Bicarbonato de Sódio
8.70 ± 0.057 B
Sensodyne Cool Gel
60.85% D
Sensodyne Original
7.81 ± 0.011 D
Triclosan-containing dentifrices
Triclosan-containing dentifrices
Colgate Total 12
46.99% A
Colgate Total 12
7.76 ± 0.029 C
Sensodyne Proteção Total
40.92% B
Sensodyne Proteção Total
8.36 ± 0.055 A
Close-Up Gel
38.21% C
Close-Up Gel
7.15 ± 0.040 B
Prevent Anti-Placa
55.16% D
Prevent Anti-Placa
6.33 ± 0.066 D
Dentifrices containing whitening agents
Dentifrices containing whitening agents
Close-Up Whitening
44.72% A
Close-Up Whitening
7.87 ± 0.079 A
Sorriso Branqueador
39.90% B
Sorriso Branqueador
10.09 ± 0.142 B
Sensodyne Branqueador
65.83% C
Sensodyne Branqueador
9.11 ± 0.155 C
40.07% A
Colgate Sensitive Branqueador
8.00 ± 0.043 A
Colgate Sensitive Branqueador
Different letters indicate statistically significant differences between
groups (p<0.05, ANOVA and post-test Bonferroni).
Different letters indicate statistically significant differences between
dentifrices (p<0.05, ANOVA and post-test Bonferroni).
155
Characterization of dentifrices
and 40.07%, respectively).
Multiple comparisons showed that there were
statistically significant differences for almost all tested
dentifrices (Table 2). Sensodyne Branqueador dentifrice
(Group 3) showed larger amount of solid residue (65.83%).
S.C.S. Pinto et al.
Braz Dent J 25(2) 2014
Figure 1. Dentifrices containing desensitizing agents: SEM micrographs of inorganic particles. A: Colgate Sensitive; B: Sensodyne Bicarbonato de
Sódio; C: Sensodyne Cool Gel; D: Sensodyne Original.
Figure 2. Triclosan-containing dentifrices: SEM micrographs of inorganic particles. A: Sensodyne Proteção Total; B: Close-Up Gel; C: Colgate Total
12; D: Prevent Anti-Placa.
156
particles that are rather regular than irregular, which may
indicate minor abrasion.
Sensodyne Whitening: Small and regular particles,
which may indicate little abrasiveness.
Sorriso Whitening: Small, spherical and regular particles,
which may indicate little abrasiveness.
The EDX analysis showed the elements present in the
abrasive agent of each product. Dentifrices containing
calcium carbonate as abrasive agent presented calcium
(Ca) and carbon C. Dentifrices containing silica as abrasive
agent showed silicon (Si) and oxygen (O) in the EDX analysis.
Discussion
Dentifrices must be sufficiently abrasive to perform
their functions without causing damage to the teeth and
must provide maximum cleaning with minimum wear.
However, tooth structure loss may occur in the crown,
the root or in both, forming non-carious cervical lesions.
Studies on non-carious cervical lesions have reported that
risk factors for tooth abrasion include age, oral hygiene
and dentifrice (3,9).
Dentifrices are used daily by the population worldwide,
but little information is available about these products,
which would be important for dentists to recommend the
proper use to patients.
The pH of the dentifrices analyzed in this study was
neutral and basic, except for Sensodyne Cool Gel (Group
1) and Prevent Antiplaca (Group 2), which presented a
slightly acidic pH. A concern regarding the use of acidic
products is the possibility of increasing enamel wear due
to the synergistic action of erosion and abrasion during
tooth brushing (10). The alkaline pH of dentifrices helps
neutralizing acid biofilm, which can cause dental caries (11).
Some authors have reported that dentifrices with acidic
pH increase the binding of fluoride to the teeth (12,13). A
recent in vitro study showed that a 550- µg F/g acidified
dentifrice (pH 5.5) had the same effectiveness as a 1.100- µg
F/g neutral dentifrice in a pH-cycling model (7). Using the
same protocol, Alves et al. (10) found that dentifrices with
a lower pH (4.5) led to better results when compared with
those reported by Brighenti et al. (7). These data suggest
that the pH reduction leads to less mineral loss, probably
because of the formation of more CaF2 adsorbed to the
enamel surface (and therefore greater availability of F). It is
important to observe that the tested dentifrices had slightly
acidic pH, which may have little influence on the fluoride
action on the enamel surface. Johannsen et al. (14) carried
out measurements of the pH of dentifrices and observed
that those with low pH were more abrasive. However,
Figure 3. Dentifrices containing whitening agents: SEM micrographs of inorganic particles. A: Close-Up Whitening; B: Colgate Sensitive Branqueador;
C: Sensodyne Branqueador; D: Sorriso Branqueador.
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Characterization of dentifrices
Braz Dent J 25(2) 2014
S.C.S. Pinto et al.
Braz Dent J 25(2) 2014
when treating a patient with dentin exposure, acidic
pH dentifrice may have negative effects on this surface,
leading to the loss of dentine structure. Therefore, patients
with this condition need to be advised to use dentifrices
with neutral or basic pH. In a previous study (13), when
a slurry with basic pH was used after softening, a slightly
better rehardening could be measured (13). It is believed
that the manufacturers are concerned about formulating
dentifrices with higher pH to eliminate the possibility of
low pH aggravating dental structure loss by abrasion (9).
In order to understand the greater variation in
abrasiveness of different trademarks, the desiccation
loss of dentifrices was also investigated. The desiccation
loss in the present study was similar among the groups.
Sensodyne Original (64.07%), Sensodyne Cool Gel (60.85%)
and Sensodyne Branqueador (65.83%) showed greater
content of abrasive agents, but other studies found no
correlation between the content of abrasives and abrasion
degree (15,16).
The dentifrice stain-removal property is basically
related to the abrasives in its composition. It is important
to point out that if, on the one hand, increased dentifrice
abrasiveness leads to improved stain removal efficacy, on
the other hand, it increases tooth wear (16).
The quality and quantity of abrasives of dentifrices
may influence its abrasiveness. The most common abrasive
agents present in dentifrices are: calcium carbonate and
silica, although others remain present. Larger content of
abrasives may harm hard tissues, soft tissues and dental
restoration. The most common harms are: gingival recession
and cervical abrasion, both usually associated with dentin
hypersensitivity (13,17).
In the present study, silica and calcium carbonate
were observed as abrasive agents and some of dentifrices
present both of them. Most dentifrices containing silica
had smaller particles with regular shape as shown in
Figures 1-3. In the study carried out by Vicentini et al. (9),
the silica dentifrices presented the least abrasive power.
In an in situ study, Pickles et al. (18) observed that a
commercial silica dentifrice caused less dentine wear tooth
when compared with other dentifrices containing calcium
carbonate, but this wear was not significantly different.
Considering dentin surface, calcium carbonate has shown
low abrasion, which probably reflects the softness of this
material in relation to the other abrasives in dentine (5).
A previous study concluded that dentifrices with calcium
carbonate of rhombohedral or ovoid shape, a more regular
structure, present lower abrasiveness than more irregular
particles (12). Another study showed that dentifrices with
sharp particles, regardless of the abrasive agent, calcium
carbonate or silica abrasives, present lower abrasiveness
(15). It is important to remind that chemically identical
158
abrasives may have different effects and the mixture
of these abrasives may result in effects that differ from
those when the components are used individually (9). The
package and tubes of dentifrices only indicates the main
type of abrasive contained in the formula, but the shape
and size of particles are not mentioned. It reinforces the
need of further studies on the dentifrice abrasiveness
so that dentists may recommend the best one for each
patient’s specific need (13).
Particle size and shape are also found to influence
abrasion, particularly when comparing abrasives made
from the same compound, as silicon dioxide (artificial silica)
(15). This study presented some dentifrices with irregular
and large particles, demonstrating greater abrasiveness.
Sensodyne Cool Gel, Close Up Gel, Close Up Whitening
showed greater and more irregular particles, a feature
that may indicates a high capacity of abrasion. Therefore,
Sensodyne Cool Gel showed acid pH and a greater content of
abrasives (60.85%), features that may turn these dentifrices
not recommended for patients with gingival recession.
A dentifrice to be recommended should follow an
individual evaluation of each patient’s need (19). However,
it seems to be more reasonable that people should use less
abrasive dentifrices (13).
This study addressed some features of dentifrices, which
is an important step for recommending the ideal dentifrice
for each patient considering the individual oral condition.
Low pH, high desiccation loss and solid residue analysis,
in addition to irregular and large particles are important
characteristics to assume a more abrasive capacity of a
dentifrice. However, if one considers a patient with high
caries activity, the indication of an acidic dentifrice is
valid as a source of fluoride to bind on tooth surface.
Considering the results presented in this study, the next
step is to evaluate dentifrices with different characteristics
on tooth surface (enamel and dentin) and their abrasive
capacity under clinical conditions on toothbrushing.
Resumo
Dentifrícios com diferentes composições estão disponíveis no mercado,
mas existe pouca informação sobre suas propriedades. O objetivo do
presente estudo “in vitro” foi avaliar as características físico-químicas
de 12 dentifrícios divididos em 3 categorias, como contendo: agentes
dessensibilizantes, triclosan ou agentes clareadores. Perda por dessecação/
análise de resíduos: 5 g do dentifrício foi pesado cinco vezes para cada
grupo. Análise do pH: foram diluídos 5 g do dentifrício suspensos em
três partes de água destilada e analisados usando um potenciômetro
digital. Microscopia eletrônica de varredura (MEV): análise das cinzas,
forma e tamanho de partículas dos agentes abrasivos. Espectroscopia
de raios X por dispersão em energia (EDX): identificação dos elementos
abrasivos. Análise dos dados: Os dados foram analisados usando ANOVA
e teste pos-hoc Bonferroni (α=0,05). Perda por dessecação: 38,21% à
65,83%. Os dentifrícios contendo triclosan e agentes dessensibilizantes
mostraram diferença significante entre eles (p<0,05). Dentifrícios
clareadores mostraram diferença significante entre Close-Up Whitening
e Sensodyne Branqueador (44,72% e 65,83%, respectivamente). A maioria
dos dentifrícios apresentaram pH básico ou neutro. Diferentes formas e
tamanhos das partículas foram observadas na análise em MEV. Elementos
abrasivos foram identificados no EDX. Estes resultados demonstram que
os dentifrícios avaliados apresentaram diferentes propriedades e que suas
composições influenciam diretamente em características, resultando em
ações mais ou menos abrasivas sobre a superfície do dente. O conhecimento
sobre as características dos dentifrícios é importante para indicar o
produto ideal para cada caso.
Acknowledgements
The authors thank the Brazilian research funding agency CAPES for the
financial support.
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Received April 9, 2013
Accepted February 25, 2014
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