979 D3000 new imprint Word template Vol 13, No 1 (2025) ISSN 2167-8677 (online) DOI 10.5195/d3000.2025.979 http://dentistry3000.pitt.edu Fluoride Release of New Bioactive Orthodontic Adhesive with Color Change and Fluorescent Property Mohammed Thanoon Younis, Neam Fakhri College of Den*stry, University of Mosul, Iraq Abstract Objec8ve: This study aimed to assess the effect of adding fluorescent dyes & color change dyes in different concentraMon to bioacMve orthodonMc adhesive on fluoride release. Mate- rial and Methods: We used BioacMve BEAUTIFIL Injectable XSL (S-PRG), from (Giomer, Shofu, Japan) mixed with color change dye, Black changing to Colorless, (Atlanta chemical engineer- ing, USA). 0.02%, 0.2% and 2% of weight concentraMons were tested and with fluorescence dye (StronMum aluminate), and White Glow in the Dark Powder (Techno Glow Inc., USA), using in 5%, 10% and 15% of weight concentraMons. For fluoride release, 40 samples pre- pared and divided into 4 groups with 10 samples as following: Group 1: BEAUTIFIL Injectable XSL Adhesive (control group), Group 2: BEAUTIFIL Injectable XSL with 0.02% color change material and 5% fluorescence material. Group3: BEAUTIFIL Injectable XSL with 0.2% color change material and 10% fluorescence material. Group 4: BEAUTIFIL Injectable XSL with 2% fluorescence material and 15% fluorescence material. fluoride Ion SelecMve Electrode. Eu- tech ION 2700. ( Thermo Fisher scienMfic inc. Singapore) used to measure the release of fluo- ride ion. Results: The use of dyes with bioacMve adhesive showed staMsMcally significant dif- ferences. There was a decrease in fluoride ion with increase dye concentraMon. Conclusion: Acceptable fluoride ion release within bi- oacMve adhesive with color change and fluorescence properMes was obtained but with increase concentraMon of dyes the ion release decreased. Open Access Cita%on: Younis MT, et al. (2025) Fluoride Release of New Bioac%ve Orthodon%c Adhesive with Color Change and Fluorescent Property. Den%stry 3000. 1:a001 doi:10.5195/d3000.2025.979 Received: July 3, 2025 Accepted: July 4, 2025 Published: August 21, 2025 Copyright: ©2025 Mahmood AA. This is an open access ar%cle licensed under a Crea%ve Commons ATribu%on Work 4.0 United States License. Email: Mohammedhanoon@uomosul.edu.iq Introduc)on Orthodontic treatment involves using 3ixed or removable appliances to correct the posi- tions of teeth. Fixed appliance treatment is a traditional and widely used form of ortho- dontic treatment to correct malpositions of the teeth and occlusal discrepancies [1,2]. The movement of teeth is achieved by forces generated and directed to the teeth via arch wires and brackets [3]. During the active treatment, the arch wires are changed as the treatment progresses, but the brackets re- main attached to the enamel for the whole active treatment period. A wide variety of or- thodontic adhesives are available for the bonding brackets and orthodontic attach- ments [4,5]. Resin adhesives are a good choice for orthodontic bonding as they have good mechanical and aesthetic properties and low failure rates. Orthodontic adhesives should provide suf3icient strength to retain the appliance during treatment and allowing its easy removal at the end [6]. Patients with 3ixed orthodontic appliances show increased risk of white spot lesions (WSL) [7] and caries due to dif3iculty in maintaining oral hygiene [8,9]. Attempts were made to reduce enamel de- mineralization by introducing 3luoride re- leasing adhesives [10], e.g. amorphous cal- cium phosphate (ACP) containing adhesives [11]. We tested Light Bond from Reliance company, Transbond Plus Adhesive from 3M Unitek company [12], glass ionomer and resin modi3ied glass ionomer [13], 3luoridate varnish [14], and topical 3luoride agents [15]. Another solution proposed by research teams is introduction of bioactive glass (BAG) into the composition of orthodontic adhesives [16]. Bioactive glass material included the Gio- mers, as a surface pre-reacted glass core (S- prg). It helps prevent and treat white spots lesions [17]. Giomers are useful in the pro- cess of collating orthodontic brackets with mechanical properties like composite resins and it offers protection against carious le- sions [18]. S-prg releases various ions (3luo- ride, sodium, silicate, aluminum, borate and strontium ions that provide multiple biolog- ical functions, including the release and Fluoride Release of New BioacMve OrthodonMc Adhesive with Color Change and Fluorescent Property Vol 13, No 1 (2025) DOI 10.5195/d3000.2025.979 http://dentistry3000.pitt.edu 2 recharge of 3luoride, anti-plaque, anti-bio- 3ilm effects and pH modulation that provid- ing protection against caries [19]. Another problem associated with orthodon- tic adhesive is the presence of excess of ad- hesive escaping from under the bracket base which promotes the accumulation of food debris and creates favorable area for bacte- rial collection which led to facilitating the de- mineralization and formation of WSL [20,21]. The solution turned out to be introduce ad- hesive characterized by a contrasting color before cross-linking, which facilitates re- moval of the excess prior to curing, e.g. Transbond Plus (3M Unitek, USA), and Grengloo and Blugloo (Ormco Corporation, USA) [22]. Color change adhesive is manu- factured by adding chromatic indicators, which facilitate the visibility of excess ortho- dontic adhesive around orthodontic brack- ets before bonding procedure [23]. This color characteristic allowed the operator to see the adhesive 3lash around the bracket base and remove it before it polymerized [24]. The third problem associated with ortho- dontic treatment is debonding [25], Leaving the remnant of orthodontic adhesive on the enamel surface facilitates plaque and dental caries formation [26]. Also, using rotating dental instruments to remove the remaining white or transparent adhesive can cause damage to tooth enamel [27]. To overcome this problem, fluorescent or- thodontic adhesive has been developed to improve the visibility of the remaining adhe- sive after debonding by using ultraviolet light [28,29]. Fluorescent additives will facil- itate the discrimination between the enamel and remnants of the adhesive. This modifica- tion can maximize the preservation of tooth structure after debonding procedure [30]. The aim of this research was to evaluate the effect of adding color change and 3luorescent dies to bioactive composite to be used as an orthodontic adhesive by evaluate the degree of conversion. Materials and Methods This study was conducted at Mosul Univer- sity, Dentistry College, Dental Hospital Cen- tral Laboratory and was approved by the Ethics Committee of College of Dentistry, Mosul University, Iraq (under the code UoM.Dent.23/49). To measure 3luoride release, 40 samples of the tested materials (10 sample for each group) were used: Group 1: BEAUTIFIL Injectable XSL Adhesive (control group) Group2: BEAUTIFIL Injectable XSL with 0.02% color change material and 5% flourcence material. Group3: BEAUTIFIL Injectable XSL with 0.2% color change material and 10% flourcence material. Group4: BEAUTIFIL Injectable XSL with 2% color change material and 15% flourcence material. Plastic cylinder molds measuring 4 mm in di- ameter and 2 mm in height were used to con- struct the specimens for each group. Cellu- loid mylar strips and glass slides were placed over the mold's top and bottom surfaces. as at room temperature, the adhesive then put within the mold. The central of samples were pressed between a celluloid strip and a glass cover slip and placed in plastic mold rings to extrude the excess material, to obtain a smooth 3lat surface, to prevent air bubble formation & to prevent oxygen layer for- mation. Then light cure the materials by us- ing LED with at 1500 mw/cm2 were cured from the top & bottom for 20sec. After light curing, each set specimen was released from the mold and placed into a polyethylene test tube. 3illed with 5 ml of deionized water. Af- ter that, each test tube was sealed, labelled, and arranged as previously indicated before being kept for 24 hours at 37°C with 95% rel- ative humidity [31=-33]. Fluoride measurements were performed on 1st day (24 h), 7 days (1 week), and 30 days (1 month). All of the samples were main- tained at 37°C in a incubator throughout the experiment. In this examination before test- ing the containers were thoroughly shaken and the specimens removed, washed, re- turned and immersed into a new 5 ml of fresh deionized water fresh solution. Mean- while, the 3luoride ions concentration in the storage media was measured. The 1st meas- urement was done after 24 h from sample preparation, and then 24 hours before day 7th and day 30th. The storage medium was changed with new 5 ml of fresh deionized water fresh solution every 24 h to avoid cu- mulative effects and because it is possible that the medium may get saturated with the released 3luoride ions, preventing further 3luoride ion release. This was done by using a 3luoride Ion Selective Electrode (Eutech ION 2700 meter, Thermo Fisher Scienti3ic Inc., Singapore) attached to an ion selective electrode meter. For statistical analysis, the amount of 3luoride in each solution was measured and recorded as part per million (ppm). Before and after each measurement, the electrode tip was washed and lightly dried with deionized water to remove any residual 3luoride ions which may affect the measurement [34,35] (Figure 1). Results Fluoride release values are represented in units of part per million (ppm) and shown in Table 1. The analysis of variance of one way (ANOVA) test for each group revealed signif- icant differences (p≤0.05). Discussion Fluoride is clearly known as an anti-caries agent, and 3luoride release is an important part of restorative materials, 3luoride can help reduce tooth decay by reducing bacte- rial metabolism and increasing the re- sistance of enamel and dentin [36,37]. Gio- mer is one of modern restorative material that contain in its chemical structure combi- nation of 3luoroaluminosilicate glass, poly- alkenoic acid and water, with resin included. What differentiates giomer from other 3luo- ride-containing restorative materials is that they contain a pre-reacted glass (S-PRG) 3iller in their matrix. This 3iller facilitates the release of 3luoride ions [35,38]. Due to the absence of an acid-base reaction, giomer ma- terials do not have a glass ionomer matrix phase. The quantity of 3luoride released by giomer materials was discovered to be less than that of GIC since they only include S- PRG particles as a 3luoride component. The materials' antibacterial properties rely on metal ions such aluminum, strontium, zirco- nium, and barium in addition to the 3luoride that is emitted [39,40]. Numerous studies shown that giomer possesses physical quali- ties that might compete with other compo- site resin, as well as a high 3luoride release and rechargeability [41]. The quantity of wa- ter absorbed, the giomer's porosity, the 3iller, the water content, the solubility of ytterbium tri3luoride in water, and the resin's permea- bility all affect how many ions are released from the giomer [42]. Giomer has a 3luorine concentration of only 4.13% [43]. Fluoride release from the material is im- portant due to the formation of 3luorapatites as well as the anti-caries property that can prevent the formation of microorganisms. The smallest quantity of 3luoride that must be released to inhibit demineralization and promote the remineralization has not been precisely determined [44]. Some authors re- ported that this value would be between 0.02 and 0.06 ppm [45]. Others said that 0.2 ppm signi3icantly reduces the risk of dental caries lesions [46]. Fluoride released from the restorative mate- rial reduced the solubility of dental tissue in acidic environments, this property being based on the 3luoride capacity to incorporate itself into the crystalline structure of the hy- droxyapatite of the dental hard tissue, result- ing in a mineral phase which was less soluble & more resistant to the cariogenic challenge. So, since enamel solubility is low when 3luo- ride ions are present in saliva & bio3ilm, it is desirable to select dental materials with the highest & longest 3luoride release [47,48]. Fluoride Release of New BioacMve OrthodonMc Adhesive with Color Change and Fluorescent Property Vol 13, No 1 (2025) DOI 10.5195/d3000.2025.979 http://dentistry3000.pitt.edu 3 Many methods have been employed to esti- mate the sum of fluoride releases such as spectrophotometry, ion chromatography, fluoride ion-specific electrodes and capillary electrophoresis [49]. Ion-specific electrode with an ion analyzer was used in this study because it is simple, inexpensive and does not require the use of complex laboratory equipment. Also, it gives an accurate and di- rect estimate of the free fluoride present in the solution [50]. To measure the 3luoride release of restora- tive materials, a variety of media, including deionized water, arti3icial saliva and acidic media, may be selected. Since deionized wa- ter is readily available & contains no ions, it is believed that 3luoride release may be more accurately quanti3ied. For this aim, deionized water used in our research protocol to be consistent with previous investigations [48,51]. In this study, we can see two events. One, it is related with decrease the rate of 3luoride release with time for all groups. So, the 1st day show the highest rate then followed by 7th day while the 30 day show the lowest 3lu- oride rate. The 2nd one related to the groups was that the control group (adhesive only) showed the highest followed by adhesive +5% 3luorescence+0.02% color change, then adhesive +10% 3lourcence +0.2% color change and 3inally adhesive +15% 3luores- cence +2% color change showed the lowest 3luoride release rate. These occurred due to the many reasons; one of them related to the time, it because to the statement that 3luo- ride release drop with time due to the mech- anism of its release as suggested by many au- thors. According to this mechanism, S-PRG is composed of three layers: a multifunctional glass core is the innermost layer, followed by a glass ionomer phase from the acid-base re- action that contains the polyacrylic acid chain and ions trapped in the phase, and the surface-modi3ied layer (porous inorganic sil- ica glass layer) at the outermost layer. Diffu- sion of the 3luoride ion from the intermediate layer to the environment is the mechanism of 3luoride release. A 3luoride ion is traded for a hydroxyl ion in an ion exchange process, which is the primary mechanism of 3luoride ion release in giomers [52]. The complex process of 3luoride ion release is in3luenced by both internal and external factors, including the type and permeability of the 3illing material, the frequency of 3luo- ride exposure, the type and concentration of the 3luoridating agent, temperature, prepa- ration method, material solubility, composi- tion, powder-liquid ratio, surface area of the specimen, matrix, 3iller composition, storage medium, saliva composition and acidity and the type and concentration of the 3luoridat- ing agent. The precise quantity of 3luoride released, which inhibits demineralization and encourages remineralization, is un- known. However, since 3luoride ions in the oral cavity decrease enamel solubility, it is better to utilize materials with a high and sustained 3luoride ion release [53-55]. Although the exact mechanism behind the ion release from S-PRG 3iller is unknown, it is thought that the existence of a glass ionomer phase around the 3iller's glass core is con- nected to the ion release [56]. Fluoride was released from the surface in a burst in the 3irst step, which is followed by a signi3icant reduction in elution and a second bulk diffusion process that releases minute quantities of 3luoride into the surrounding medium. Fluoride is thus released on the 3irst day due to a surface rinsing impact and on following days its diffusion via pores and fractures is responsible for the release. For the 3luoride ions to diffuse, the resin mono- mer gradually absorbs water [57,58]. So, in the 3irst phenomenon of 3luoride re- lease called the “Burst Effect”. The second bulk diffusion phase, which releases 3luoride in minute quantities via the material matrix pores, occurs concurrently with the later slow release. This could have to do with the kind of 3illers used. Another aspect may be the bonding between the matrix and the 3ill- ers. It was discovered that more microporos- ities may have resulted from the dye parti- cles' inability to connect with the adhesive matrix, which might have facilitated the re- lease of 3luoride which agrees with Bansal & Bansal in 2015 & Dawood et al in 2019 [57- 59]. It is shown that giomers have a lower 3luoride release than glass ionomers, with no early 3luoride burst impact, but that 3luoride release levels are mostly constant. The initial intense release of these ions may also be due to surface leaching, while its subsequent sta- bilization results from the diffusion of 3luo- ride ions through the pores and fractures of the material [38,58]. Additionally, the ionic interaction on the sur- face of the glass particles or water absorp- tion after the dissolution of the glass 3iller particles might cause 3luoride release [60]. In addition, the 1st step of 3luoride released from the surface of giomer after which the elution is markedly reduced, accompanied by the second bulk diffusion process by which small amounts of 3luoride continue to be released into the surrounding media [61]. As during water penetration through diffu- sion, the surface layers will be more satu- rated than the inner mass leading the mate- rial can leach ions from the mass that have been penetrated by water & the penetration of water is different for different materials, depending on the permeability of materials [62,63]. Anyway the release of 3luoride from giomer is more water-exposure dependent [64]. When the S-PRG encounters water, the ions that are not bonded in the polymeriza- tion chain created in giomer are dissolved. For example, the polymer in the giomer will react to create a polymer chain when ex- posed to light. Many ions that are not part of the polymer chain are present in the polymer chains in order for them to dissolve in the immersion solution. Fluoride is one of the ions not included in this polymer chain [42,65]. The results of this study agree with Sang- eetha in 2005 who approved that the fluo- ride release rate was maximum at 1st day then subsequently dropped to a lower level after one week and had reached a near con- stant level at 30th day [66]. Salmerón-Valdés et al in 2016 said, in vitro, the degree of fluo- ride released from giomer was maximum during the 1st 24 hs, then after 8 days showed minimum levels of released fluoride [67]. Ga- roushi et al (2018) who calculated the daily release of fluoride over a period of 10 days from bioactive materials, he said that fluo- ride start to decrease from 1st day with until the 10th day [48]. Also Nahum et al in 2021 said that all materials analyzed in his study demonstrate the greatest fluoride release in the first 24 h, followed by a marked decrease after 5th days (68). Feiz et al in 2022 approve that the supreme mean of fluoride released during the days 1st, 3rd, and 7th then decrease on day 14th [37]. Pastrav et al in 2021 and Marnani & Kazemian 2024 suggested in their studies that the dental materials which re- lease fluoride ions show highest activity on the 1st day after setting, followed by a grad- ual decrease in the number of ions released over the following days, months and years [34,69]. Harhash et al in 2019 discovered that after the first day, the commercial gio- mer Beautifil Flow Plus F03, A2 color, emit- ted 1.0020 ppm of fluoride, 0.4140 ppm after the first week, and 0.3165 ppm after the fourth week [42]. While Rusnac et al in 2021, according to his research, the experimental giomer emitted 1.87 ppm of fluoride after the first day, 0.766 ppm after a week, and 0.307 ppm after 30 days. Fluoride levels in the giomer B-F03 were 3.1 ppm after the first day, 0.442 ppm during the first week, and 0.242 ppm after 30 days [70]. While in the other side like Zabokova et al in 2011 said that the amount of fluoride after 3 & 6 months it was higher compared to initial values this may be due the material & tech- nique that he used it in his research [71]. The second phenomena occur due to the many reasons one of them is the presence of 3iller within constant sample lead to de- crease the size of adhesive which leading to decrease the quantity of 3luoride in the testes sample when compare with the control sam- ple. However, other writers hypothesized Fluoride Release of New BioacMve OrthodonMc Adhesive with Color Change and Fluorescent Property Vol 13, No 1 (2025) DOI 10.5195/d3000.2025.979 http://dentistry3000.pitt.edu 4 that the high degree of conversion from a double to a simple bond, which results in the cohesiveness of polymer networks and low- ers the mobility of ions like 3luoride, might be the cause of the reduced release. A double bond's high degree of conversion to a single bond (–c=c-) (c–c). which mean that increase in polymerization would result in entrap- ment of 3luoride ions inside the lattice of the polymer, so the amount of 3luoride release will be decreased [72,73]. This can be disa- greeing with our results related with DC, this may be due to the difference between size of samples & presence of dyes 3iller that pro- duce some voids within mixture leading to release 3luoride from this voids this agree with Alinda et al (2021) who said, voids play a signi3icant role in releasing 3luorine ions [40]. Al-Shekhli & Al_Aubi in 2020 said that incor- poration of 3iller in the composition of gio- mer restorative material tend to be affected by water exposure more than other 3iller types incorporated in restorative [74]. Jita- luk et al. (2022) implied that adding 20 weight percent nano3illers to resin improved the 3luoride exchange compared to using mi- cro3illers at the same amount [35]. The difference in our result of 3luoride re- lease from results in another studies may be related to the difference in the type and size of material also due to the difference in the type and size of storage media that used this agree with Burtea et al. (2019) [52]. Anyway, the decrease in the 3luoride release rate can be raised by 3luoride recharge as suggested by Barakat & Abdelrahim in 2022, who claimed that after being exposed to 3luoridated chemicals, the giomer could be recharged and re-release 3luoride gradually [50]. Giomer can be recharged with 3luoride ions by topically applied NaF gel and 3luori- dated toothpaste () (64). Finally, the quantity of 3luoride that is re- leased from the specimens cannot be antici- pated to be the same as what happens within the mouth. The true effectiveness of restora- tions can only be ascertained by long-term clinical trials, even if laboratory investiga- tions are crucial for providing quick answers to certain concerns & It should also be con- sidered that the results were obtained in ex- perimental conditions that cannot com- pletely reproduce the conditions of the oral environment this agree with Naoum et al (2012) & Gateva et al (2023) [38,75]. 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Naoum, S., O’Regan, J., Ellakwa, A., Benkhart, R., Swain, M., & Martin, E. (2012). The effect of re- peated Fluoride recharge and storage media on bond durability of Fluoride rechargeable Giomer bonding agent. Aust Dent J. 57(2): 178-183. 76. Senthilkumar, A., Chhabra, C., Trehan, M., Pra- dhan, S., Yadav, S. and Shamsudeen, N.H. (2022). Comparative evaluation of Fluoride release from glass ionomer, compomer, and giomer sealants fol- lowing exposure to Fluoride toothpaste and Fluoride varnish: an in vitro study. Intern J Clinic Pedia Dent. 15(6): 736-738. Figure 1. Samples used to test 3luoride release. Table 1. Fluoride release values in ppm for all groups. Groups N Time Minimum Maximum Mean Std. Deviation Control 10 24 h 1.64 1.74 1.67 0.0374 7 day 1.49 1.57 1.53 0.0251 30 day 1.47 1.51 1.49 0.0139 5%+0.02% 10 24 h 1.60 1.72 1.66 0.0368 7 day 1.49 1.62 1.52 0.0365 30 day 1.43 1.51 1.48 0.0244 10%+0.2% 10 24 h 1.54 1.66 1.61 0.0442 7 day 1.43 1.59 1.51 0.0463 30 day 1.40 1.50 1.47 0.0294 15%+ 2% 10 24 h 1.54 1.64 1.59 0.0316 7 day 1.47 1.57 1.51 0.0319 Fluoride Release of New BioacMve OrthodonMc Adhesive with Color Change and Fluorescent Property Vol 13, No 1 (2025) DOI 10.5195/d3000.2025.979 http://dentistry3000.pitt.edu 7 Table 2. Duncan's analysis for determining the difference between the groups. Groups Time 1 2 3 4 5 6 7 8 9 10 Control 24hrs 1.73 1.65 1.64 1.65 1.68 1.74 1.64 1.64 1.65 1.68 7 days 1.55 1.57 1.54 1.51 1.49 1.54 1.55 1.54 1.52 1.5 30 days 1.49 1.49 1.51 1.47 1.48 1.51 1.49 1.51 1.48 1.49 5%+0.02% 24hrs 1.62 1.67 1.68 1.7 1.66 1.6 1.67 1.68 1.72 1.63 7 days 1.5 1.53 1.54 1.49 1.52 1.5 1.62 1.53 1.52 1.51 30 days 1.49 1.5 1.5 1.47 1.46 1.46 1.51 1.49 1.49 1.43 10%+0.2% 24hrs 1.64 1.65 1.64 1.54 1.59 1.65 1.66 1.65 1.55 1.6 7 days 1.58 1.51 1.43 1.49 1.53 1.59 1.52 1.5 1.49 1.54 30 days 1.49 1.46 1.4 1.48 1.5 1.5 1.47 1.48 1.46 1.49 15%+ 2% 24hrs 1.6 1.59 1.54 1.58 1.64 1.61 1.61 1.55 1.59 1.63 7 days 1.56 1.51 1.49 1.5 1.48 1.57 1.52 1.51 1.52 1.47 30 days 1.51 1.45 1.48 1.48 1.44 1.52 1.46 1.42 1.48 1.43