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Communication

Design and Characterization of Non-Erosive Polymeric Tooth-Whitening Compositions

by
Dohyuk Yoo
*,
Jae-Hyun Ahn
and
Nae Gyu Kang
LG Household and Health Care R&D Center, Seoul 07795, Republic of Korea
*
Author to whom correspondence should be addressed.
Appl. Sci. 2023, 13(6), 3698; https://doi.org/10.3390/app13063698
Submission received: 6 February 2023 / Revised: 7 March 2023 / Accepted: 13 March 2023 / Published: 14 March 2023
(This article belongs to the Section Applied Dentistry and Oral Sciences)
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Abstract

:
We investigated the physical properties and tooth-whitening effect of polymeric tooth-whitening compositions based on orally acceptable polymers, polyvinyl acetate (PVAc), ethyl cellulose (EC), and polyvinyl pyrrolidone. The tooth-whitening composition was prepared with hydrogen peroxide (H2O2) as a tooth-bleaching agent and an orally acceptable polymer through simple mixing and stirring in ethyl alcohol. PVAc and EC polymers showed non-erosive features and sustainable polymeric matrices in a similar oral environment. In particular, non-erosive PVAc polymer exhibited excellent adhesive and flexible film matrix on bovine teeth. PVAc-H2O2 tooth-whitening composition presented a residual H2O2 and an overall color change value (ΔE*) of 26.5% and 16.54%, respectively. The non-erosive polymeric composition is expected to improve tooth-whitening efficacy in various oral products.

Graphical Abstract

1. Introduction

Hydrogen peroxide (H2O2) is widely used as an antiseptic, hydrolysis, and bleaching agent in various industries, including the pharmaceutical and household [1,2,3]. The whitening mechanism of H2O2 typically involves the decomposition of H2O2 into hydroxyl radicals and the oxidation of stained organic matters by hydroxyl radicals [2,4]. Teeth whitening products with the aforementioned mechanism are applied to the stained substances in the oral cavity to perform teeth bleaching [2]. Generally, various peroxide types, including the aqueous solution of 30–50% H2O2 [2,3] and carbamide peroxide [5], are applied in tooth whitening. However, a concentration of 30–50% H2O2 solution is extremely irritating for direct application as a tooth-bleaching agent. Hence, it is diluted up to 0.25–15% and mixed with various additives, such as orally acceptable polymers, surfactants, and stabilizers, to produce tooth-whitening compositions [6,7].
Considerable research has been conducted on tooth-whitening compositions. Reinhardt et al. investigated the whitening effects of four types of whitening protocols: toothpaste, whitestrips, bleaching agents, and polishing application [7]. Ren et al. studied the effects of 6% H2O2 whitening composition with a LED light on the enamel surface and compared it with that of the orange juice [8]. Meireles et al. evaluated the influences of three concentrations of carbamide peroxide, which are used for tooth bleaching [9]. Among numerous studies on teeth whitening, gel-type whitening compositions containing H2O2 are extensively studied. Sulieman et al. evaluated the whitening effectiveness according to H2O2 concentrations [10]. Acuna et al. investigated the effectiveness of bleaching gels in offices at different pH values [11]. Consequently, gel-type tooth-whitening compositions are easy to use at home or in-office and suitable for examining various effectiveness.
Oral care products, such as tooth-whitening composition, are manufactured by combining various raw materials, such as orally acceptable polymers, solvents, fragrances, and stabilizers. Orally acceptable polymers with H2O2 are available in several grades, such as polyvinyl pyrrolidone (PVP) [12], cellulose derivatives [13,14], and (meth)acrylates copolymers [14]. Among these, polyvinyl acetate (PVAc) is commonly used as a bio-adhesive and film-forming agent in various industries, including food and pharmaceutical and has been reported to be safe as a cosmetic component [11,14,15]. Ethyl cellulose (EC) is also a water-insoluble material that can be applied to the oral cavity such as coating agent [14]. Additionally, PVP exhibits excellent solubility in many solvents such as water and alcohol and provides H2O2 stability through hydrogen bonding between the carboxyl group of PVP and H2O2 [16]. Primeval PVAc and EC demonstrate alcohol-soluble and non-erosive properties in water phase. Therefore, they can be utilized in oral care products with appropriate contents of water and additives. Moreover, PVAc maintains good water resistance and can sustainably release active substances, such as H2O2, in the oral environment [17,18].
In this study, tooth-whitening compositions were designed using PVAc, EC, and PVP as polymeric matrices for delivery of active substances, such as H2O2, for tooth whitening. In addition, their characterization and whitening efficacy were investigated.

2. Materials and Methods

2.1. Materials

H2O2 solution (35% food grade H2O2) was purchased from OCI Company Ltd. (Seoul, Republic of Korea). PVAc (VINNAPAS® B 100 SPECIAL, Wacker Chemie AG, Munich, Germany), EC (Aqualon EC-N22 Pharm, Ashland, DE, USA), and PVP (Plasdone™ k-29/32, Ashland, DE, USA) were obtained from the respective suppliers. A concentration of 99.5% ethyl alcohol (EtOH), ammonium molybdate tetrahydrate ((NH4)6Mo7O24·4H2O), and sodium thiosulfate standard solution (0.05 N, Na2S2O3) were purchased from Daejung Chemicals & Metals Co., Ltd. (Gyeonggi, Republic of Korea). Potassium iodide solution (1.0 N KI, Fisher Chemical, Waltham, MA, USA) and sulfuric acid (95.0–98.0% H2SO4, ACS Reagent, Sigma-Aldrich, Munich, Germany) were purchased from the respective suppliers. All solvents and reagents were used as received without further purification. Deionized (DI) water was obtained from Milli-Q® Direct Water Purification System (Merck Millipore, Burlington, MA, USA, 7.1 µS/cm conductivity) with a pH of 6.0 to 7.0 and was applied to all use in this study. Bovine teeth were obtained from a private butcher’s shop (only enamel parts, Hanwooga, Seoul, Republic of Korea).

2.2. Characterization

The surface morphology of the whitening compositions was investigated by atomic force microscopy (AFM, XE-100, Park Systems/PSIA, Suwon, Republic of Korea) and digital optical microscopy (DOM, BX53MTRF-S, OLYMPUS, Tokyo, Japan). The thermal properties of glass as a function of temperature were determined using differential scanning calorimetry (DSC 4000, PerkinElmer, Waltham, MA, USA) in air. The color change (ΔE) was examined using a spectrophotometer (NF555, Nippon Denshoku, Tokyo, Japan).

2.3. Preparation of Tooth-Whitening Compositions

A non-erosive polymer (PVAc or EC, 20 g) was directly added to EtOH (72 g) and stirred at 25 °C for 3 h. Next, 35% H2O2 solution (8 g) was slowly added to this solution as a bleaching agent to prevent the aggregation of the polymer and H2O2. After sufficient mixing, the non-erosive tooth-whitening compositions PVAc-H2O2 and EC-H2O2 were obtained (Figure 1). The PVP-H2O2 tooth-whitening composition was also prepared similarly using PVP.

2.4. Fabrication of Polymeric Tooth-Whitening Composition Films

Glass microscope slides (Paul Marienfeld GmbH & Co. KG, Lauda-Königshofen, Germany) were prepared as substrates by sequential washing with acetone, ethanol, and distilled water for 10 min each to remove any impurities and then dried in a convection oven at 100 °C for 30 min. A blue dye (SunCROMA FD&C, Sun Chemical®, Parsippany-Troy Hills, NJ, USA, 0.01 g dye per 100 g of whitening composition) was added to the prepared compositions and stirred for 30 min. The prepared polymeric tooth-whitening compositions were then deposited on a glass substrate via casting. A film of the polymeric tooth-whitening composition was annealed on the glass substrate at 25 °C for 1 h.

2.5. Contact Angle Measurements

The coated films were prepared by dip-coating glass slides with PVAc-H2O2, EC-H2O2, and PVP-H2O2 tooth-whitening compositions. A drop of distilled water (approximately 0.3 μL) was deposited on the coated film before the air–water contact angle was measured.

2.6. Optical Microscopy and Glass Transition Temperature Measurements

Bovine teeth have already been removed from all impurities at the butcher’s shop, and only enamel parts of bovine teeth specimen have been obtained. The obtained teeth were washed 10 times or more in streaming water, and then they were dried at room temperature for one day. Each tooth-whitening composition (approximately 0.1 g) was applied on bovine teeth using a brush applicator and dried for 1 min before viewing under an optical microscope. The bovine teeth were subsequently immersed in distilled water at 37 °C for 1 h. To measure glass transition temperature of polymers, polymer specimen containing 0.01 g of pristine polymer and a reference specimen were prepared, and the changes in heat flow were determined at a rate of 5 degrees per minute from 0 to 200 °C.

2.7. Residual H2O2 of Tooth-Whitening Compositions (In-Vitro)

The durability of tooth-whitening compositions was assessed by measuring the residual amount of H2O2 on bovine teeth over time. The bovine teeth have already been removed from all impurities at the butcher’s shop of “Hanwooga”, and only enamel parts of bovine teeth specimen have been obtained. The whitening compositions (20 μL) were applied to the surfaces of separate bovine teeth specimens. The coated bovine teeth were then immersed in water (25 mL) at 37 °C for 30 min and 1 h. Subsequently, the bovine teeth were transferred in ethanol (50 mL), and the concentration of H2O2 was determined by a potassium iodide thiosulfate titration using (NH4)6Mo7O24, Na2S2O3, KI, and H2SO4; the titration was conducted five times to obtain an average value [19,20]. The residual H2O2 results were calculated using a statistical tests, one-way analysis of variance (ANOVA) [6]. ANOVA is a statistical method used to compare the means of three groups. It determines whether there is a meaningful difference between group means based on the variation within each group and the variation between groups. For comparisons between experimental groups, we performed a Bonferroni post hoc test. Differences were assumed to be significant if the p-value was less than 0.05 (significant codes; *: p < 0.05, **: p < 0.01, ***: p < 0.001).

2.8. Whitening Effect of Tooth-Whitening Compositions (In-Vitro)

A whitening evaluation of hydroxyapatite (HAP) specimens stained with coffee and other contaminants was conducted by the Stookey method to confirm the whitening ability of the compositions [21]. After measuring the initial color intensity of the stained HAP specimens using a colorimeter, the whitening compositions (50 μL) were applied to separate HAP specimens. The whitening HAP specimens were soaked in water at 37 °C for 1 h and dried in a convection oven at 50 °C before the color intensity was measured. L*, a*, and b* are symbols for the CIELab color space, where L* means brightness, with L* = 0 for black and L* = 100 for white. a* exhibited the red (+a*), green (−a*), and b* represents yellow (+b*) and blue (−b*). The L*, a*, and b* values measured after the treatment of the HAP discs were compared with those measured before the treatment to define the whitening effects in accordance with CIELab to determine the overall color change (ΔE*) quantitatively [22]. The experiment was repeated ten times to obtain an average value. The variable results of overall color changes were also estimated using statistical tests—one-way ANOVA complemented with the post hoc Bonferroni test [6].

3. Results and Discussion

3.1. General Manufacture of Polymeric Tooth-Whitening Compositions

Polymer material in the whitening composition must have negligible water solubility to retain its whitening properties in the oral environment. Hence, common polymers with low water solubility, such as PVAc and EC were used. For comparison, a control sample was also prepared in a same manner using PVP, which is a water-soluble polymer widely used in oral products. All solutions and films of the prepared tooth-whitening compositions exhibited a single, homogeneous phase (Figure S1a).

3.2. Durable Water Resistance of Tooth-Whitening Compositions

The prepared PVAc-H2O2, EC-H2O2, and PVP-H2O2 tooth-whitening compositions and the corresponding films coated on glass slides were colorless and homogeneous. Hence, to evaluate the water resistance of the PVAc-H2O2 and PVP-H2O2 tooth-whitening compositions, the test specimens dyed blue and coated on a glass slide were prepared, as described in the experimental section (Figure S1b). The PVP-H2O2 film, which contained the highly water-soluble PVP polymer, was washed off the glass slide (Figure 2). In contrast, the non-erosive PVAc-H2O2 and EC-H2O2 films showed very high retention, with no loss relative to their initial [23,24]. These results suggest that the non-erosive tooth-whitening compositions will not be washed away in the oral environment and will be retained for a long time.
The change in contact angle was measured to evaluate the water resistance of PVAc-H2O2, EC-H2O2, and PVP-H2O2 tooth-whitening compositions (Figure 3). The initial contact angle of 32.4° in the PVP-H2O2 tooth-whitening composition sharply decreased to 9.8° after 120 s, and the PVP film could not be maintained owing to its water solubility. Conversely, the PVAc-H2O2 and EC-H2O2 tooth-whitening compositions initially had high contact angles of 60.6° and 65.1°, respectively, which changed to 56.4°, 61.7°, respectively, after 120 s. Furthermore, the PVAc-H2O2 and EC-H2O2 polymer films did not erode over time, allowing their contact angles to be maintained.

3.3. Surface Morphologies and Film Features of Tooth-Whitening Compositions

The surface morphology of the PVAc-H2O2, EC-H2O2, and PVP-H2O2 tooth-whitening compositions on bovine teeth were examined by DOM and AFM. The initial coating surfaces of the whitening composition exhibited uniform morphologies (Figure 4). After 1 h treatment, the surface morphology of the PVAc-H2O2 remained the same as before, owing to its high adhesion [23,25]. Conversely, EC-H2O2 was partially removed, leaving a brittle film texture on the surface of the bovine teeth.
Pristine PVAc, EC, and PVP polymers were verified using DSC to estimate the glass transition temperatures of the films (Figure S2). The glass transition temperature (Tg) of PVAc (45.1 °C) was lower than that of the EC and PVP 74.1–134.8 °C and 116.1 °C, respectively [26,27,28]. In general, the oral temperature range was 33.2–38.2 °C [29]. PVAc film with the glass transition temperature closest to the oral temperature range was expected to be more flexible than EC and PVP films.
The AFM images revealed a smooth coating of PVAc-H2O2 on the bovine tooth surface (Figure 5a). After drying, a uniformly coated surface was obtained without any observable clumps or agglomeration. The parameters of average roughness (Ra) and root-mean-square roughness (Rq) of the coating side were 7 nm and 14 nm, respectively. The coating on the tooth was peeled off using a double-sided tape and observed by AFM to examine the surface of the tooth coating on the attachment. Unlike the coating on the tooth surface, the film of the tooth-whitening composition coated on the attachment side exhibited pseudo-isomorphic morphology with the bovine tooth surface. The Ra and Rq of the attachment side were 135 nm and 168 nm, respectively. The pristine bovine teeth surface exhibited Ra and Rq values of 123 nm and 154 nm, respectively (Figure S2). The obtained AFM images confirmed that the PVAc-H2O2 tooth-whitening composition coated on the surface of the bovine teeth retained its initial morphology (Figure 5b). Additionally, the coated film has specific surface morphology and excellent wettability and, hence, is expected to exhibit a significant tooth-whitening effect [30,31].

3.4. Residual H2O2 of Tooth-Whitening Compositions (In Vitro)

The residual H2O2 concentrations on the bovine teeth were measured by potassium iodide thiosulfate titration experiments to confirm the sustainability of the coated whitening compositions (Figure 6) [19,32,33]. Significant difference (p value) between the means of the whitening composition groups exhibits Tables S1–S3. The initial H2O2 concentrations in the non-erosive PVAc-H2O2 and EC-H2O2 tooth-whitening composition were 2.88% and 2.82%, respectively. The residual H2O2 concentrations in PVAc-H2O2 on the coated bovine teeth were 1.48% and 0.76% at 30 and 60 min, respectively, while those of the EC-H2O2 composition were 1.39% and 0.55% at 30 and 60 min, respectively. Conversely, the initial H2O2 concentration in the PVP-H2O2 tooth-whitening composition was 2.86%, while the residual H2O2 concentrations in the PVP-H2O2 coated bovine teeth were 1.26% and 0.37% at 30 and 60 min, respectively. Thus, after 1 h, the PVAc-H2O2 and EC-H2O2 tooth-whitening compositions retained 26.5% and 19.5% H2O2 with respect to the initial concentrations, whereas the PVP-H2O2 tooth-whitening composition retained only 12.9% H2O2 compared to the initial concentration. The non-erosive PVAc-H2O2 tooth-whitening composition showed 2.05 times higher retentions of H2O2 on bovine teeth than the PVP-H2O2 tooth-whitening composition. Therefore, a more effective tooth-whitening effect is expected because the coating persists for a longer time without being eroded in oral environment.

3.5. Whitening Effects of Tooth-Whitening Compositions (In-Vitro)

ΔE values derived from the CIELab color space were the difference between the initial values. [34] To evaluate the in vitro whitening effects of the tooth whitening composition, L*, a*, and b* were measured under the initial condition of the HAP specimen and after 1 h of H2O2 treatment, and the ΔE values were measured and calculated in Table 1, Table S4, and Figure 7 [35,36]. Additionally, the significant difference (p value) between the means of the whitening composition groups is exhibited in Table S4. The ΔE values of the HAP specimens treated with the non-erosive PVAc-H2O2, EC-H2O2, and erosive PVP-H2O2 tooth-whitening compositions for 1 h were 16.54, 9.91, and 6.97, respectively. The color changes in the PVAc-H2O2 tooth-whitening composition were 40.8% higher than that in the PVP-H2O2. Furthermore, the PVAc-H2O2 composition exhibited significantly enhanced tooth-whitening efficacy than EC-H2O2 and PVP-H2O2. The PVAc-H2O2 tooth whitening composition did not easily wash off the coated surface, resulting in an excellent whitening effect for HAP samples. On the other hand, the EC-H2O2 composition was not easily washed, but the adhesive force to the coated surface was weaker than PVAc-H2O2 composition, resulting in a lower whitening effect. The PVP-H2O2 tooth whitening composition was not water resistant and was easily erased, so the whitening effect was low. Therefore, the non-invasive PVAc-H2O2 tooth whitening composition was predicted to be maintained for a longer period without being washed out in the oral environment. In addition, H2O2 is predicted to be retained more effectively on the tooth surface than other products that can be washed off by water, thereby maximizing the whitening effect. However, bleaching agents have been demonstrated to have a significant influence on bond strength of glass ionomer cements [37] and composites [38], but further studies are needed in order to complete the overview about their effects in clinical dentistry.

4. Conclusions

The non-erosive polymeric tooth-whitening composition PVAc-H2O2 exhibited whitening effects superior to that of PVP-H2O2 composition in a similar oral environment. The PVAc-H2O2 tooth-whitening compositions exhibited high water resistance, adhesion, and flexible films. Consequently, the PVAc-H2O2 composition is expected to achieve an excellent tooth-whitening performance owing to its high retention and low erosion in the oral environment. Unfortunately, this research was only experimented with in the in vitro study, and whether non-erosive polymeric teeth whitening compositions can indeed achieve enhanced whitening effects in the actually oral cavity requires further study.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/app13063698/s1, Figure S1: Photo images of tooth whitening composition solutions and films coated on slide glass [dip coating method] (a) pristine solutions and films, (b) adding dye in solutions and their films; Figure S2: Thermal properties of pristine polymers (a) PVAc, (b) EC and (c) PVP; Figure S3: AFM surface morphology of pristine bovine teeth surface; Table S1: Residual H2O2 concentration of polymeric whitening compositions (initial); Table S2: Residual H2O2 concentration of polymeric whitening compositions (exposed 30 min); Table S3: Residual H2O2 concentration of polymeric whitening compositions (exposed 60 min); Table S4: L* a* b* and ΔE values of initial and H2O2 treated conditions for whitening compositions.

Author Contributions

Conceptualization, D.Y. and J.-H.A.; methodology, D.Y.; validation, D.Y.; investigation, D.Y.; writing—original draft preparation, D.Y.; writing—review and editing, D.Y. and J.-H.A.; visualization, D.Y.; supervision, N.G.K.; project administration, J.-H.A. and N.G.K. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The data presented in this study are available in [Supplementary Material here].

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. Illustration of manufacturing process of polymeric tooth whitening composition.
Figure 1. Illustration of manufacturing process of polymeric tooth whitening composition.
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Figure 2. Photograph of dyed tooth whitening samples dipped in water during 60 min.
Figure 2. Photograph of dyed tooth whitening samples dipped in water during 60 min.
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Figure 3. Contact angle plot and photo-images of PVAc-H2O2, EC-H2O2 and PVP-H2O2 compositions coated on slide glass; (a) initial, (b) after 120 s.
Figure 3. Contact angle plot and photo-images of PVAc-H2O2, EC-H2O2 and PVP-H2O2 compositions coated on slide glass; (a) initial, (b) after 120 s.
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Figure 4. Digital optical microscopy images of initial and dipping 60 min of tooth whitening compositions coated on bovine teeth: (a) PVAc-H2O2, (b) EC-H2O2, and (c) PVP-H2O2.
Figure 4. Digital optical microscopy images of initial and dipping 60 min of tooth whitening compositions coated on bovine teeth: (a) PVAc-H2O2, (b) EC-H2O2, and (c) PVP-H2O2.
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Figure 5. AFM surface morphology of PVAc-H2O2 tooth whitening composition; (a) coating side and (b) attachment side of bovine teeth.
Figure 5. AFM surface morphology of PVAc-H2O2 tooth whitening composition; (a) coating side and (b) attachment side of bovine teeth.
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Figure 6. Residual H2O2 concentration of PVAc-H2O2, EC-H2O2 and PVP-H2O2 tooth whitening compositions. (significant codes; *: p < 0.05, **: p < 0.01, ***: p < 0.001).
Figure 6. Residual H2O2 concentration of PVAc-H2O2, EC-H2O2 and PVP-H2O2 tooth whitening compositions. (significant codes; *: p < 0.05, **: p < 0.01, ***: p < 0.001).
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Figure 7. ΔE values of various polymeric tooth whitening compositions after 1 h of treatment (in vitro). (significance codes; ***: p < 0.001).
Figure 7. ΔE values of various polymeric tooth whitening compositions after 1 h of treatment (in vitro). (significance codes; ***: p < 0.001).
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Table
Table 1. Contact angle, residual H2O2 concentration, and whitening effect of polymeric tooth-whitening compositions.
Table 1. Contact angle, residual H2O2 concentration, and whitening effect of polymeric tooth-whitening compositions.
Polymeric
Tooth-Whitening Compositions		Contact Angle (°)Residual H2O2 Concentration (%)In-Vitro
Whitening
Effect (ΔE*) 1
Initialafter 120 sInitial30 min60 min
PVAc-H2O260.656.42.88 (±0.05)1.48 (±0.17)0.76 (±0.17)16.54 (±5.33)
EC-H2O265.161.72.82 (±0.11)1.39 (±0.18)0.55 (±0.12)9.91 (±2.30)
PVP-H2O232.49.82.86 (±0.21)1.26 (±0.13)0.37 (±0.04)6.97 (±0.82)
p value 0.7960.1769.24 × 10−53.16 × 10−6
1 ΔE* value of blank specimen without tooth whitening composition is 1.10 (±0.37).
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Yoo, D.; Ahn, J.-H.; Kang, N.G. Design and Characterization of Non-Erosive Polymeric Tooth-Whitening Compositions. Appl. Sci. 2023, 13, 3698. https://doi.org/10.3390/app13063698

AMA Style

Yoo D, Ahn J-H, Kang NG. Design and Characterization of Non-Erosive Polymeric Tooth-Whitening Compositions. Applied Sciences. 2023; 13(6):3698. https://doi.org/10.3390/app13063698

Chicago/Turabian Style

Yoo, Dohyuk, Jae-Hyun Ahn, and Nae Gyu Kang. 2023. "Design and Characterization of Non-Erosive Polymeric Tooth-Whitening Compositions" Applied Sciences 13, no. 6: 3698. https://doi.org/10.3390/app13063698

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