Journal of Oral Rehabilitation 2002 29; 791798

Fluoride release and uptake characteristics of aesthetic restorative materials

NEN N. ATTAR & A. O
Faculty of Dentistry, Department of Conservative Dentistry, University of Hacettepe, Ankara, Turkey

SUMMARY The aims of this study were rstly to investigate the uoride-releasing characteristics of two composite resins (Tetric and Valux Plus), two polyacid-modied resin composites (Compoglass and Dyract), and conventional glassionomer cement (Ceraml b). The second aim was to assess the uoride uptake and subsequent release from the same range of materials. Fifteen discs (6 mm diameter and 15 mm height) were prepared for each material. Each disc was immersed in 4 M L of deionized water within a plastic vial. The release of uoride was measured daily at 1, 2, 3, 4, 5, 15, 30 and 60 days. After daily uoride release was measured for 60 days, samples were reuoridated in 1000-ppm sodium uoride (NaF) solutions (pH 66) for 10 min and uoride release was measured daily for a total of 5 days. The release of uoride from aesthetic restorative materials was measured by

using specic uoride electrode and an ionanalyser. Results were statistically analysed by two-way repeated measure ANOVA and Duncans multiple range test. The results revealed that all uoridecontaining materials (Ceraml b, Compoglass, Dyract, Tetric) released uoride initially and the release was greatest at the rst day. At any time during the test period Ceraml b released the most and Valux Plus did not release any detectable uoride (P < 001). Sample exposures to 1000 ppm NaF solution increased the 24-h uoride release from all uoride-containing materials. This difference lasted only 2448 h after exposure. Ceraml b had a tendency to recharge not seen with the other materials (P < 005). KEYWORDS: glassionomer cement, polyacid-modied resin composite, composite resin, uoride release, uoride uptake

Introduction
Replacement of restorations because of secondary caries is a continuing problem in restorative dentistry. The ability of a restorative material to resist secondary caries and microleakage at its margins will, to a great extent, determine whether a restoration will succeed or fail (Dionysopoulos et al., 1998). Development of an ideal restorative material, that provides a permanent seal with tooth structure, has been thwarted by complicating factors present in the oral environment: changes in intraoral temperature (thermal expansion), solubility of certain restorative materials in saliva and change in pH (Olsen et al., 1989; Donly & Ingram, 1997). Consequently, increased emphasis has been placed on developing restorative materials with anticariogenic properties.
2002 Blackwell Science Ltd

Fluoride has demonstrated anticariogenic effects and this benecial effect on the human dentition has led to the examination of available uoride in a host of dental materials (Rawls & Zimmermann, 1983; Skartveit, Tveit & Extrand, 1985; Olsen et al., 1989; Forsten, 1991; Donly & Ingram, 1997; Dionysopoulos et al., 1998). Glassionomer cements were rst introduced to the dental profession by Wilson and Kent in 1972. Their main characteristics are an ability to chemically bond to enamel and dentine with insignicant heat formation or shrinkage; biocompability with the pulp and periodontal tissues; uoride release producing a cariostatic and antimicrobial action (Rawls & Zimmermann, 1983; Skartveit et al., 1985; Olsen et al., 1989; Forsten, 1991; Donly & Ingram, 1997; Dionysopoulos et al., 1998; Hse, Leung & Wei, 1999). Many investigators have demonstrated the ability of glassionomer to increase the

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uoride content in enamel and dentine adjacent to restorations (Retief et al., 1984; Forss & Seppa, 1990; Skartveit et al., 1990). The uptake of uoride would increase its resistance to acid demineralization and prevent caries formation around restorations (Retief et al., 1984; Hicks, Flaitz & Silverstone, 1986; Forss & Seppa, 1990; Skartveit et al., 1990; Tyas, 1991; Varpio & Noren, 1994; Donly & Ingram, 1997; Dionysopoulos et al., 1998). Fluoride release from glassionomers also has an antimicrobial action against Streptococcus mutans in plaque (Seppa, Torppa-Saarinen & Luoma, 1992; Benelli et al., 1993; Seppa, Korhonen & Nuutinen, 1995). In the late 1980s and early 1990s, a couple of so-called light cured glassionomers were released in the market. From a chemistry point of view there are two different routes towards these hybrid materials (Guggenberger, May & Stefan, 1998). These include the resin-modied glassionomer cements and the polyacid-modied resin composites (compomers). Resin-modied glassionomer materials were basically formed by adding methacrylate derivatives to the glassionomer formula. Both laboratory and clinical research has clearly demonstrated the ability of the resin-modied glassionomers to release uoride (Momoi & McCabe, 1993; Forsten, 1995; Burgess et al., 1996; De Araujo et al., 1996; Tam, C han & Yim, 1997). The uoride release from and uptake by the resin-modied products was higher than or the same as that of conventional glassionomers (Momoi & McCabe, 1993; Forsten, 1995; Burgess et al., 1996; De Araujo et al., 1996; Tam et al., 1997). Compomer means that the material possesses a combination of the characteristics of both composites and glassionomers, but actually it shows minimal glassionomer reactions (Suljak & Hatibovic-Kofman, 1996; Guggenberger et al., 1998). Polyacid-modied resin composites were formed by adding acidic polymers to the original methacrylate resin matrix. Compomer is being marketed for use as a restorative alternative to glassionomer cements. Composite resin restorations are in constantly increasing demand. However, these restorations have been associated with the occurrence of marginal secondary caries relating mainly to marginal leakage and plaque retention (Van Dijken, 1986; Wilson, Wilson & Smith, 1988). Studies of the uoridereleasing properties of composite resins indicate a long-term release of uoride, although the amount released is low in comparison with that of the glass ionomers (Swift, 1989; Young et al., 1996). In vitro studies have also shown the ability of conventional glassionomer materials and resinmodied glassionomer cements to take up uoride and subsequently release it again (Hatibovic-Kofman & Koch, 1991; Creanor et al., 1994, 1995; Forsten, 1995; Suljak & Hatibovic-Kofman, 1996; Young et al., 1996). There have, however, been few studies into the longterm uoride release from the polyacid-modied resin composites and uoride-releasing composite resins. Forsten (1998) has measured both release and uptake from both types of materials. It was mentioned that the uoride treatment had no effect on polyacid-modied composites or uoride containing composites or the amalgams. The aims of this study were rstly to investigate the uoride-releasing characteristics of two composite resins, two polyacid-modied resin composites (compomers) and conventional glassionomer cement. The second aim was to assess the uoride uptake and subsequent release from the same range of materials.

Materials and methods

The ve aesthetic restorative materials were used in this study and their characteristics are listed in Table 1. Two of the materials used were composite resins: one of them was a non-uoride-releasing composite resin Valux Plus*, and the other was uoride-releasing composite resin Tetric. The other two were the polyacid-modied resin composites Compoglass and Dyract. The last one was the conventional glass ionomer cement, Ceraml b.

Sample preparation Fifteen test samples of each material were in the form of round disc-shaped samples, 6 mm in diameter and 15 mm thick made using Teon moulds, placed between two glass plates. All restorative materials were prepared according to the manufacturers instructions using the scoops provided. The light cured materials (Compoglass, Dyract, Tetric and Valux Plus*) were cured on both sides with a Translux EC Kulzer light
*3M, Malakoff, France. Vivadent Ets, Schaan, Liechtenstein. Dentsply\De Trey, Konstanz, Germany. EC Kulzer & Co, GmbH D-6383 Wehrheim/TS Germany. 2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 791798

FLUORIDE RELEASE AND UPTAKE

Table 1. Materials tested for uoride release Restorative material Ceraml b Compoglass Dyract Tetric Valux Plus

793

Material class Conventional glassionomer cement Polyacid-modied resin composite Polyacid-modied resin composite Fluoride-releasing composite resin Non-uoride-releasing composite resin

Manufacturer PSP Belvedere, Kent, UK Vivadent Ets, Schaan, Liechtenstein Dentsply\De Trey, Konstanz, Germany Vivadent Ets, Schaan, Liechtenstein 3M, Malakoff, France

Batch No. 0694236 800647 9511060 618661 70-2010-1302-9

source for 30 s. Ceraml b was chemically setting. Samples were weighed in order to verify standardization within each material test group (001). The samples were stored at 100% relative humidity for 24 h.

with 4 mL of fresh deionized water and incubated. Fluoride release was measured daily for a total of 5 days.

Statistical analysis Two-way repeated measure analysis of variances (ANOVA s) were then performed to compare types of materials for each time point. Also two-way repeated measure ANOVA s were performed to compare time points. Statistical analysis of two-way repeated measure ANOVA on restorative material versus time revealed statistically signicant difference, so we examined consequent differences between mean values. A one-way ANOVA was performed to mean difference values of each ve groups. Duncans multiple range test were performed to identify group differences for each ANOVA .

Initial uoride release Each sample was placed in a polyethylene test tubes lled with 4 mL of deionized water. The polyethylene test tubes were incubated for 24 h at 37 C. Following incubation of 24 h, the samples were grasped with clean metal forceps and rinsed with 1 M L deionized water over the original holding tube, thus collecting the rinse water in that tube. Each disc was transferred to a new polyethylene test tube containing 4 mL deionized water and stored at 37 C. Fluoride release was determined at 1, 2, 3, 4, 5, 15, 30 and 60 days after buffering the solution with equal volumes of total ionic strength adjustment buffer (TISAB). Fluoride release was measured with a uoride ion specic electrode (Orion 96-09 electrode) and an ionanalszer (Orion EA 940). Data concerning uoride was recorded in parts per million (ppm). The electrode was previously calibrated with standards whose molarity spanned the actual concentrations of uoride to be measured (001, 01, 05, 10, 50, 100, 200 and 300 ppm). The uoride concentration was determined by adding 5 mL TISAB to each 5 mL sample solution.

Results
Fluoride release (ppm) at days 1, 2, 3, 4, 5, 15, 30, 60 and uoride release after recharging at days 1, 2, 3, 4 and 5 are presented in the Table 2. An analysis of two-way repeated measure ANOVA indicated signicant differences in uoride release among all ve materials (F 647208, P < 001). There were statistically signicant differences between all the groups. The conventional glassionomer cement (Ceraml b) was signicantly higher than all other groups, at any time during the test period. Ceraml b released the most, and Valux Plus did not release any detectable uoride. Statistical analysis of two-way repeated measure ANOVA on restorative material versus time revealed statistically signicant difference (F 103076, P < 001). All uoride containing materials released most uoride after the rst 24 h and this uoride release continued over the entire 60 days testing period. Initial uoride release decreased with time.

Fluoride release after exposure to sodium uoride (NaF) Following 60 days of initial uoride release, samples from each product were exposed to a standard solution containing 1000 ppm uoride ion made from 526 mmol L1 NaF. After copious rinses in deionize water, each sample was returned to a container lled

Orion Research Inc., Beverly, MA, 01915-6199, USA.

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NEN N. ATTAR & A. O

Statistical analysis of two-way repeated measure on restorative material versus time revealed signicant difference so we examined consequent differences between mean values. Differences between groups are shown in Table 3. There was statistically signicant difference between Ceraml b compared with all other groups (P < 005). Tables 2 and 3 shows the effects of exposures to 1000 ppm NaF solution. The rst day after exposure there was an increase in uoride releasing from all uoride containing materials. This lasted for only 2448 h after exposure. Ceraml b had a tendency to recharge not seen with the other materials. There were signicantly differences after exposure to NaF between Compoglass and Tetric at day 1day 60 and day 2day 1 and also between Compoglass and Valux Plus at day 1day 60 and day 2day 1. There was no statistically signicant difference between the polyacid-modied resin composite and between the composite resin with regard to exposure to NaF or not (Table 3). Figure 1a shows the uoride release of Ceraml b from day 1 to day 60 on the basis of the average of the 15 samples. Figure 1b shows the initial uoride release of test materials except Ceraml b from day 1 to day 60, on the basis of the average of the 15 samples. Figure 2a shows the uoride release from Ceraml b after exposure to 1000 ppm NaF solution. Figure 2b shows uoride release from the other test materials after exposure to 1000 ppm NaF solution.
ANOVA

Day 5 Day 4 Day 3 Day 2 Day 1 Day 60 Day 30 Day 15 Day 5 Table 2. Fluoride release from materials tested (ppm) (mean and s.d.)

597 048 028 005 003

062 005 004 001 001

488 051 030 003 024 004 004 00 003 000

253 054 024 005 019 003 003 00 003 001

181 040 023 003 017 002 003 00 002 000

1084 104 040 016 003

111 016 004 005 001

423 035 021 006 003

052 007 003 001 001

333 029 019 004 003

040 004 004 001 001

252 021 014 003 002

028 003 005 001 001

205 018 011 003 003

019 004 002 001 001

Day 4

066 005 004 022 000

Discussion
There were some differences in uoride release among the products, and they could represent a valid parameter to guide the selection of a material for specic clinical situations. Kan, Messer & Messer (1997) suggested that each individual product should be independently tested to evaluate the amount of uoride that can released. Fluoride release from glassionomer appears to be much greater than from either uoride containing amalgam or composite (Forsten, 1990). However, glassionomer cements are not widely used as a restorative material. Their lack of acceptance may be a result of their technique sensitivity to moisture, low mechanical strength and wear resistance (Burgess et al., 1996; Guggenberger et al., 1998). The uoride release of conventional glassionomer cements has been attributed to acidbase setting reactions involving
2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 791798

Day 3 Day 2 Groups Day 1

Ceraml b 2753 213 Compoglass 237 021 Dyract 097 006 Tetric 055 008 Valux Plus 004 001

1439 163 073 032 003

210 022 005 004 001

1090 095 059 015 003

095 010 006 003 001

686 059 038 017 003

FLUORIDE RELEASE AND UPTAKE

uoride-containing glasses and a polyacid liquid (Smith, 1990). This results in the large surge of ion release in the rst few days as the material sets and the majority of glass species react. In agreement with previous studies this experiment showed that the greatest uoride release occurred during the rst 24 h, diminishing to a signicantly lower level the next day. This result is in accordance with the other studies reported by El Mallakh and Sarkar (1990), and also De Schepper et al. (1991). The high concentration observed in the rst days are called the burst effect of the uoride. The reason for the rapid fall in uoride release is likely to be the result of the initial burst of uoride released from the glass particles as they dissolve in the polyalkenoate acid during the setting reaction. The later slow release occurs as the glass dissolves in the acidied water of the hydrogel matrix (De Moor, Verbeeck & De Maeyer, 1996). The mean uoride release of ve aesthetic restorative materials shown as an example in Fig. 1a, b, reveals the initial burst effect of Ceraml b and the release remaining at a certain constant level for 60 days. However, polyacid-modied resin composites (compomers) and uoride-releasing composite resin did not show an initial uoride burst effect. In the present study, Compoglass and Dyract released signicantly less uoride initially than did the conventional glassionomer cement (Ceraml b), because the rst phase of setting is essentially the same as that occurring when resin composites are cured. The initially light cured material takes up water with time, and the carboxylic groups (COOH) of the acidic monomer can undergo an acid/base reaction with metal ions of the glass ller. This, in turn, leads to the formation of carboxylate salts and the release of uoride (Dentsply De Trey, 1996). It seems that this reaction is weak and results in low uoride release. This material behaves more likely as a resin composite than like glassionomer cement in terms of uoride release (Suljak & Hatibovic-Kofman, 1996; Yip & Smales, 1999). In this study, Compoglass and Dyract in fact seem to follow a similar pattern to Ceraml b in having the highest release in the rst day and having progressively less uoride release as time progresses. The second part of the experiment also showed that all uoride containing materials released, increased the amounts of uoride on exposure to uoride followed by a rapid return to near pre-exposure levels already
Groups Day 2Day 1 Day 3Day 2 Day 4Day 3 Day 5Day 4 Day 15Day 5 Day 30Day 15 Day 60 Day 30 Day 1Day 60 Day 2Day 1 Day 3Day 2 Day 4Day 3 Day 5Day 4 030 006 005 001 001

795

* * * * * * * * 235 006 005 001 000 * * * * 076 006 005 001 001 072 000 003 000 001 * * * * 082 004 004 001 001 903 080 024 013 001 134 016 004 022 001 661 068 019 010 000

121 017 005 023 002

089 007 002 003 000

* * * * * * * *

Table 3. The mean values of consequent differences among groups and the results of signicance test

Differences

076 006 004 001 001

081 008 005 001 001

* * * *

034 003 007 001 001

047 003 003 000 001

* * * *

2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 791798

A B C D E AB AC AD AE BC BD BE CD CE DE

*P < 005. (A) Ceraml b, (B) Compoglass, (C) Dyract, (D) Tetric, (E) Valux Plus.

1314 074 024 024 001 * * * *

233 349 032 069 009 014 009 016 001 000

* * * *

254 025 007 005 001

404 035 021 002 000

* * * *

118 010 007 022 001

089 011 010 012 000

* * * *

096 008 006 022 001

109 018 005 001 000

* * * *

090 006 005 001 001

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NEN N. ATTAR & A. O

Fig. 1. (a) Initial uoride release of Ceraml b. (b) Initial uoride release of other test materials (ppm).

Fig. 2. (a) Fluoride release from Ceraml b after exposure to 1000 ppm NaF solution. (b) Fluoride release from the other test materials after exposure to 1000 ppm NaF solution.

within 3 days. Dyract and Compoglass exhibited a signicantly lower reuoridation-release property than did the one conventional glassionomer material tested. Dyract and Compoglass act more like a resin composite than like a glassionomer cement with respect to uoride uptake (Burgess et al., 1996; Suljak & Hatibovic-Kofman, 1996). In the present study, Dyract seems to follow a somewhat different shape plot to Compoglass. Compoglass, a product that contains specic uoride compounds besides the uoride containing reactive glass showed somewhat higher values than Dyract. Compoglass released relatively more uoride than Dyract. However, there were no statistically signicant differences between Dyract and Compoglass with regard to exposure to NaF or not (P < 005). The uoride values of the uoride containing composite resin (Tetric) decreased to almost zero after the fth day. Laboratory studies have shown that

glassionomer cements can be recharged but that resin composites cannot (Hatibovic-Kofman & Koch, 1991; Burgess et al., 1996). Arends and Ruben (1988) found that uoride is released from a resin composite but to a much lesser extent than is released from a glassionomer cement. It seems that uoride compounds added to the composition of composite resin lead to low uoride release. The increased uoride release after exposure of Tetric, Compoglass, Dyract to 1000 ppm uoride are most probably because of surface-retained uoride. Compoglass, Dyract and Tetric released uoride in such small quantities that little or no recurrent caries inhibition would be expected. However, precise minimal uoride concentrations for caries inhibition have not been established (Swift, 1989). Even a small amount of uoride leaching might provide some cariostatic effect if sustained for a long time.
2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 791798

FLUORIDE RELEASE AND UPTAKE

With regard to clinical criteria, the recharge could still be an important factor as the recharged cements. Frequent application of relatively low concentrations of uoride will eliminate caries, even in situations of high caries challenge (Toumba & Curzon, 1993). The levels of long-term uoride ion release from dental materials are more important than the transient levels of any initial bursts and it is important to follow the release pattern until the steady-state level is reached. Some studies have been conducted on the long-term uoride release from glassionomer cements (Forsten, 1990). Aged glassionomer cements can be recharged with topical uoride treatment (Forsten, 1991) and can act as slow release systems to apply uoride directly to tooth structure (Hatibovic-Kofman, Koch & Ekstrand, 1997). The amount of uoride released in the present study was determined in a neutral environment; however, uoride release is increased by lowering the pH of the storage medium (De Araujo et al., 1996). In the oral environment this could be the case especially with a plaque induced acidogenic challenge. Normally, under acidic conditions such as found under established plaque, there is an increased uoride release from glassionomer materials. Previous studies have shown evidence for this behaviour (Forsten, 1991). It has been postulated that the increased uoride release at pH 5, as compared with neutral pH may be caused by the undesirable, faster dissolution of the lling material (Forsten, 1991). During this research, the uoride ions were collected in distilled water instead of articial saliva. El Mallakh and Sarkar (1990) have shown that the release into articial saliva is less compared with deionized water but, in that study no account was taken of presence of plaque or pellicle which may also concentrate uoride levels. The clinical signicance of the released uoride is yet to be fully conrmed. Many factors, such as the site into which the uoride diffuses and the rate of dilution, will inuence its anticaries effectiveness. The property of glassionomers, resin-modied glassionomer cements, polyacid-modied resin composites and composite resins, however, to take up and release extrinsic uoride would indicate that this mechanism may be able to take place in vivo. The ultimate goal of correlating uoride release with actual caries reduction is an objective that can only be met by completing controlled clinical studies on
2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 791798

797

materials with well-characterized kinetics of uoride release.

Conclusions
1. All uoride containing materials tested (Ceraml b, Compoglass, Dyract, Tetric) demonstrated the ability to release uoride initially. At any time during the test period Ceraml b released the most and Valux Plus did not release any detectable uoride. 2. All uoride containing materials released the greatest amount of uoride in the rst day following sample preparation. 3. Samples exposure to 1000-ppm NaF solution increased the 24 h uoride release from all uoride containing materials. This difference lasted only 24 48 h after exposure. Ceraml b had a tendency to recharge not seen with the other materials.

Acknowledgments
This work was partly supported by the grants from Hacettepe University Research Fund (97.T01102025) and The Scientic and Technical Research Council of Turkey (SBAG-1804).

References
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Correspondence: Dr Nuray Attar, 8 Cadde Buket Apartments, 62A Daire: 12, 06510 Emek Ankara, Turkey. E-mail: nurayattar@hotmail.com

2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 791798