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(1)Title. Spectral Characteristics of Light-curing Units and Dental Adhesives. Author(s) Alternative. Kameyama, A; Hatayama, H; Kato, J; Haruyama, A; Teraoka, H; Takase, Y; Yoshinari, M; Tsunoda, M. Journal. Journal of Photopolymer Science and Technology, 24(4): 411-416. URL. http://hdl.handle.net/10130/2533. Right. Posted at the Institutional Resources for Unique Collection and Academic Archives at Tokyo Dental College, Available from http://ir.tdc.ac.jp/.

(2) Spectral Characteristics of Light-curing Units and Dental Adhesives Atsushi Kameyama1, 2*, Hitoshi Hatayama3, Junji Kato2,4, Akiko Haruyama2, Hiromi Teraoka2, Yasuaki Takase2, Masao Yoshinari1, 5 and Masatake Tsunoda2 1. Oral Health Science Center HRC7, Tokyo Dental College, 1-2-2 Masago, Mihama-ku, Chiba 261-8502, Japan 2 Division of General Dentistry, Tokyo Dental College Chiba Hospital, 1-2-2 Masago, Mihama-ku, Chiba 261-8502, Japan 3 Lightwave Network Products Division, SEI Optifrontier Co., Ltd., 1-4-1 Shimomachiya, Chigasaki, Kanagawa 253-0087, Japan 4 Cariology and Operative Dentistry, Department of Restorative Sciences, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, 1-5-45, Yushima, Bunkyo-ku, Tokyo113-8549, Japan 5 Division of Oral Implants Research, Oral Health Science Center, Tokyo Dental College, 1-2-2 Masago, Mihama-ku, Chiba 261-8502, Japan. Reprinted from. Journal of Photopolymer Science and Technology Vol. 24, No. 4, 411-416 (2011).

(3) lournqtofPhotop01ymeritienくeqndTeくhnotogy. Volume24,Number4(2011)411−416◎2011CPST. SpectralCharacteristicsofLight−CurlngUnitsand DentalAdhesives AtsushiKameyamal,2*,HitoshiHatayama3,JunjiKato2,4,AkikoHaruyama2,. HiromiTbraoka2,ⅥsuakiTakase29MasaoYbshinaril,5andMasatakelもunoda2 Jord肋dJあぶCね〃CeCe〃Jer〃尺C7,乃砂0上板〃JdCo//曙e, /一二一∴l山†(喋り.几〟/7(刷‘ノー拓(77彷‘′プ引−(Yj〃ユノ叩‘J/7. 2か油加げGe〃erdかe〃血堺乃砂0加〃gdCoJ/曙eC捕α月b岬ぬた ノー2−2几勿∫αgO,ル行毎∽α一転C加わα267−8502,ノ毎フα〃 j⊥なあ仙αVe脱仙0戒PmゐcJ∫β摘扇b〃,5gJqフ′卸〃/わrCoリムJd, 7−4−/∫/7血…JJ(J(イJ恒J.〔ソ癌(J.…鉦〟(…‘′g‘ハ…Jjj−/ノ〃〟7,ノ岬‘JJ7 JC‘J′・/前脚・‘′/7‘/q九mJ/血D川J/、咋β叩‘′′・/川川J扉▲鮎招ノ′・‘′/血∫(・/川。ハー GJ・‘J‘山‘血∫(ノ佃両村わ‘/hJ/州‘/伽77/‘J/∫ぐ/州。ぐ・V,乃木。▲lわ‘//(・“/‘肌/β川〟′/い7汗ピ/叫l−, ノー5−45,挽∫あわ刀α,β〃〃砂0−ん〟,乃砂0JJ3−854夕,ノ毎フα刀 子耕一血刷(亘り′・‘′//′叩/刷/.V月山ピ‘肛/7.0′・‘′/〃ぐ‘′仙∫(血7ぐピ(1川ナビ′:叫一・。仇′77‘′/C。//堵ぐ・ ノー2−2ル払∫dgO,脚力α∽α一五〃,C鋸α26ノー8502,ノ毎フα〃 「*ピー〃誼.・ん(川呵l川JJ(由/(わ.(′。・万り. Most manufacturers do not provide details about the photoinitiators containedin dental adhesives.Therefbre,1tis difncultto choose an optlmalcombination ofdentaladhesive and light−Curlngunit・Thepurposeofthisstudywastherefbretoinvestlgatethespectralemission characteristicsofseveralcommerciallyavailablelight−Curlngunitsandthespectraltransmittance characteristics ofcontemporary dentaladhesives・Spectraldistributions ofemittedlights were. determinedonaUV−Vis−NIRspectrometerfbrthreequartz−tungSten−halogen(QTH)light−Curing units(Jetlite3000,J.Morita;New Light VL−2,GC;D−Lux2000,Dentrade)and three light−emittingdiode(LED)light−Curingunits(Curenos,Shofu;G−LightPrima,GC;Bluephase, lvoclarVivadent).Spectraldistributionsoflighttransmittanceincontemporarydentaladhesives (ScotchbondMulti−Purpose,3MESPE;AdperSingle Bond,3M ESPE;One−Step,Bisco;AQ BondPlus,SunMedical;OptiBondA11−in−One,Kerr;ClearnlS3Bond,KurarayMedical;G−Bond, GC;Tokuyama Bond Force,Tokuyama Dental;GBA300experimental,GC)were also determined.EachofthethreeQTHlight−Curingunitshadawideemissionrangeof380−510nm・A narroweremissionrangewasobservedintheLEDlight−CuringunitsthanintheQTHlight−Curing units.Itwasfoundthat2LEDlight−Curlngunitshaddualpeakwavelengthsinboththeblueand violetreglOnSOfthevisiblespectrum・Therewere somevariationsinlighttransmittance,and therefbre the results suggested that some dentaladhesives contain altemative photoinitiators besidescamphorqulnOne・The selectionofsuitablelight−Curlngunits onthebasisofthelight absorptlOnOfdentaladhesivesandresincompositesindentalclinicsisofupmostimportance・ Keywords:light−Curlngunit?dentaladhesive?Photoinitiator†1ight−emittingdiode,. absorptionspectra,emissionspectra. 1.1ntroduction. Size),lowerpowerconsumption,longerlifb span. Recentlyanewtypeoflight−Curlngunithasbeen. andlower heat generation[3].Therefbre,the. developed that uses blue−light emittlng diodes. marketshare ofLEDlight−Curlngunitsisrapidly. (blue−LEDs)[1,2].The LEDlight−Curlng unit. growing[4].. exhibits better perfbrmance than conventional. The types of resin composite restorative. quartz−tungSten−halogen(QTH)light−Curing units. materialsthatareindemandhaverecentlychanged.. due toits portability(itis cordless and smallin. Tb meet the aesthetic needs of clients,. Received January18,2011 Accepted March 25,2011. 411.

(4) J. Photopolym. Sci. Technol., Vol. 24, No. 4, 2011. bleaching-white composites have been developed to match very light shades. Some of these composites include alternative photoinitiators such as 1-phenyl-1,2-propanedione (PPD) [5], 2,4,6-trimethylbenzoyl diphenylphosphine oxide (MAPO or Lucirin TPO) [6], and bis (2,4,6-trimethylbenzoyl)-phenylphosphine oxide (BAPO or Irgacure 819) [7], in order to avoid residual yellowing caused by camphorquinone (CQ) [8-10]. The types of resin-tooth adhesive systems that are in demand have also changed. One-step self-etch adhesives (1-SEAs) are becoming increasingly popular. Since these simplified adhesives are blended with a hydrophilic component(s) and a high concentration of solvent in hydrophobic dimethacrylates, the steps of etching, priming, and bonding can be performed simultaneously [11]. Therefore, use of these adhesives is less time consuming, and reduces the number of complicated application steps. On the other hand, it has been reported that, with respect to both enamel and dentin, these adhesives have lower bonding effectiveness and long-term bond durability than multi-step adhesives [11, 12]. One of the reasons for this has been commonly associated with their lower degree of polymerization caused by the presence of water [13]. Additionally, it is well known that the polymerization efficiency of the traditional photoinitiator CQ is considerably lower than that of alternative initiators [14-16]. Some products therefore include alternative initiators [17]. The absorption spectra of alternative initiators are distributed in the ultraviolet to violet regions and are different from those of CQ [14, 18, 19]. The use of these alternative initiators is therefore. incompatible with the narrow spectrum of blue LED light-curing units. In order to overcome this problem, several manufacturers have developed dual- or multi-wavelength LED light-curing units. Unfortunately, most manufacturers do not provide details regarding the photoinitiators contained in commercially available dental adhesives. Therefore, it is difficult to choose an optimal combination of dental adhesive and light-curing unit. The purpose of this study was, therefore, to analyze the spectral emission characteristics of several commercially available light-curing units and the spectral transmittance characteristics of contemporary dental adhesives by using an ultraviolet-visible light-near infrared (UV-vis-NIR) spectrophotometer. 2. Materials and Methods 2.1. Spectral analyses of light-curing units The setup for the spectral analysis of each light-curing unit is schematically shown in Fig. 1. Six light-curing units were evaluated for spectral analysis (Table 1). The light was directed through an optical fiber (Ocean Optics, Dunedin, FL, USA) connected to a UV-vis-NIR spectrophotometer (USB-4000, Ocean Optics), and emission spectra were determined at 0.2 nm intervals. The obtained data were recorded and analyzed on a computer connected to the spectrophotometer. Each emission spectrum was determined in three different irradiation modes in G-Light Prima. Table 1. Light-curing units used in this study Light-curing unit (Manufacturer). <Quartz-tungsten-halogen> D-Lux 2000 (Dentrade, Osaka, Japan). 412. Power density (mW/cm2). Diameter (mm). 1250. 8. New Light VL-2 (GC, Tokyo, Japan). -. 700. 11. Jetlite 3000 (J. Morita USA, CA, USA). -. 790. 11. -. 1550. 8. G-Light Prima (GC, Tokyo, Japan). Normal PL PH. 1150 52 1150. 8 8 8. Bluephase ( Ivoclar Vivadent, Schaan, Lichtenstein). High. 1120. 9. <LED> Curenos (Shofu, Kyoto, Japan). Fig. 1. Schematic illustration of the spectral measurement of light-curing unit. Mode.

(5) J. Photopolym. Sci. Technol., Vol. 24, No. 4, 2011. 2.2.. Spectral analyses of light transmittance through dental adhesives The procedure for the spectral analyses of light transmittance is schematically shown in Fig. 2. Eight commercially available dental adhesives and one experimental dental adhesive were investigated for analyses of light transmittance (Table 2). A deuterium tungsten halogen light source (DH-2000, Ocean Optics, Dunedin, FL, USA) was connected to a UV-vis-NIR spectrophotometer (USB4000) using two optical. Fig. 2. Schematic illustration of the spectral measurement of dental adhesive Table 2. Adhesives used in this study Adhesive. Manufacturer. <3-step etch-and-rinse adhesive> Scotchbond Multi Purpose 3M ESPE, St. Paul, MN, USA <2-step etch-and-rinse adhesive> Adper Single Bond 3M ESPE, St. Paul, MN, USA One-Step Bisco, Schaumburg, IL, USA <1-step self-etch adhesive> AQ Bond Plus. OptiBond All-in-One Clearfil S3 Bond. G-Bond Tokuyama Bond Force. GBA-300 (Experimental). Batch No. 7PR. 6kp 0600003472. Sun Medical, Moriyama, Shiga, Japan Kerr, Orange, CA, USA Kuraray Medical, Kurashiki, Okayama, Japan. ML2. GC, Tokyo, Japan Tokuyama Dental, Kamisu, Ibaraki, Japan GC, Tokyo, Japan. 0701131 001. 2731583 00004A. fibers separated by a sample holder. One drop of the unfilled resin was placed onto a thin glass plate (thickness: 0.15 mm; Matsunami Glass Industries, Ltd., Kishiwada, Osaka, Japan), covered with another glass plate, and gently compressed using finger pressure. Imediately afterwards, each resin sample was placed in the sample holder and irradiated with light. The light transmission spectra through each adhesive sample were acquired in 0.2 nm increments. 3. Results 3.1. Emission spectra of light-curing units The emission spectra of the light-curing units are shown in Fig. 3. Each of the three QTH light-curing units had a wide emission range of 380-510 nm. The peak wavelength of D-Lux 2000 (473.4 nm) was slightly shorter than New-Light VL-2 and Jetlite 3000 (491.0 nm). The Curenos LED light-curing unit had a narrower emission range than that of QTH light-curing units; a range of 420-510 nm with a peak in the blue region (462.9 nm). Both the normal mode and PH mode of G-Light Prima had an emission peak wavelength at 462.9 nm, which was the same as that of Curenos. However, these modes had one more peak in the violet region (402.9 nm). The peak height ratios (blue/violet) in the normal mode and PH mode were 1:0.0956 and 1:0.6265, respectively. Bluephase G2 had also two emission peaks in the blue and violet regions of the visible spectrum (410.3 nm and 454.6 nm). The peak height in the blue region was slightly lower than that in the violet region (blue/violet = 0.9455:1). G-Light Prima PL mode had only one emission peak in the violet region (402.9 nm). 3.2. Spectral characteristics of light transmittance of dental adhesives Spectra of light transmittance in each adhesive are shown in Fig. 4. Similar spectral characteristics were found in the light transmittance of Scotchbond Multi Purpose, Adper Single Bond, One-Step, OptiBond All-in-One, and Tokuyama Bond Force. Although AQ Bond Plus also had similar characteristics, the transmittance in the range of 320-350 nm was slightly lower than that of the other adhesives (arrow head). Typically shaped inverted peaks were found in the range of 355-410 nm for Clearfil S3 Bond, G-Bond and GBA 300 (pointer).. 11. 413.

(6) J. Photopolym. Sci. Technol., Vol. 24, No. 4, 2011. Fig. 3. Emission spectra of light-curing units. Fig. 4. Transmittance spectra of adhesives. The small inverse peak at 470 nm is seen in all adhesives (upper arrow). Only in AQ Bond Plus, lower transmittance zone is a transmittance drop seen in the range of 320-350 nm (arrowhead). Typically shaped inverted peaks are seen at 355-410 nm in Clearfil S3 Bond, G-Bond, and GBA 300 (pointer).. 414. 4. Discussion A conventional QTH lamp emits white light with a wide emission range between UV and NIR. In order to apply this light source in the polymerization of light-cured dental materials, unwanted wavelengths must be eliminated by placing filters between the light source and light guide so as to prevent harmful effects and pulpal damage by heat generation [20]. In this study, peak wavelength and emission range slightly differed among the three QTH light-curing units. This may be due to the different filters used. However, all these light-curing units reacted well to CQ, because the emission range and peak wavelengths of these light-curing units were almost the same as the reaction range and reaction peak wavelength of CQ. The emission range of Curenos was the same as that of a typical LED light-curing unit, and this finding was similar to that of a previous report [20]. On the other hand, G-Light Prima and Bluephase G2 employ two different LED series in the same device allowing them to operate in both blue and violet regions of the spectrum, and these devices are categorized as third-generation LED light-curing units [9, 20]. In our data, two peaks could also be found in both the violet and blue regions. However, the peak height ratios were different: G-Light Prima mainly used the blue LEDs and supplementarily used the violet LED(s) in both normal mode and PH mode. In Bluephase G2, on the other hand, blue LEDs and violet LEDs were equally used. Furthermore, the peak wavelength of its blue LED was slightly shorter than that of G-Light Prima. These differences might have an effect on curing behavior, even if the power density level is the same. In some previous studies, the absorption spectra of photoinitiators have been investigated by spectrophotometry [9, 14, 19]. However, in these previous studies, it is possible that the light absorption was not measured directly, and reflection, refraction, and scattering may have been.

(7) J・P加opo7ym・Scf・乃Cわれ07.′Vo7.24′No.4′201ユ. includedin the measurement.Therefbre,in the. COntainedanaltemativephotoinitiatorbesidesCQ.. PreSentStudy,thespectralcharacteristicsfbrlight. However,theinfluenceofthelight−Curlngunitand. transmittance through dental adhesive were determined.. dental adhesive on polymerization efnciency,. Adiplnthespectrawasobservedintherange. mechanicalproperties andresidualyellowlnghas notyetbeenclarined.Furtherstudiesaretherefbre. Of430−490nm,.WithaniTVerSePeak(入max)at around470nmlnalladhesIVeSteSted・Thismay. neededtoinvestlgatethosepolntS・. indicatethattheseadhesiyesincludeCQ・However, the reduction oftransmlttanCe WaS Small.CQis. Acknowledgments. excited to an unstable triplet state thatinteracts. Withatertlaryaminetogeneratefreeradicalsby. YoungScientistsfromMEXT,Japan((B)21791864) (A・K・)・ThisstudywasalsosupportedbyOralHealth. absorptlOnOfbluelight,andthepolymerizationof. Science Center Grant HRC7from Tokyo Dental. resin monomers caused by the breaking of. College,and. Carbon−Carbon double bonds occursl8].On the. Other hand,it is well known that the. ThisworkwassupportedbyaGrant−in−Aidfbr. by. a. HHigh−Tech. Research. Center”. PrqeCt fbr Private Universities:matChing fund SubsidyfromMEXT,Japan,2006−2010.. POlymerization efnciency of CQis verylow, because the maximum value of the molar. Refbrences. extinctioncoefncientissignincantlylowerinCQ. l・S・Nakamura,T・MukaiandM.Senoh,々n.J. than other photoinitiatorsl14−16].Recently,the micro−tenSile bond strengths of experimenta1. 1−SEAscontainingdi晩rentconcentrationsofCQ havebeen determined,andithas been concluded thatminimallyO・7wt%CQshouldbeused[21]. However,SuCh a concentration might cause undesirableaestheticeffbcts[22].. Threeinversepeakswerealsofoundat366nm, 381nmand396nminClearnlS3Bond,G−Bond andGBA300,reSPeCtively・Thepeakdistribution WaSSimilartothatofLucirinTPO[9,14,18,19, 23]・ItwastherefbrenotedthatLucirinTPOmight. beincludedintheseadhesivesasasupplementary Photoinitiator,Which not only contributes to. enhancethepolymerizationefnciencywithaQTH light source but also reduces the yellowlng Of adhesives.. ThenrstversionofAQBond(SunMedical)did notincludeCQ,butratherincludedanaltemative initiatorl24]・SinceitsabsorptionTaSdistributed. betweentheUVandvioletreglOnS,ltCOuldnotbe POlymerizedbyablue−LEDlight−Curingunit[24].. Soon after,it wasimproved to AQ Bond Plus, Which contained both CQ and the other Photoinitiator[25].Inthisstudy,thetransmittance. intherangeof330−350nmwaslowerthanthatof the adhesives which contained only CQ,Which might be due to the presence of the other. Photoinitiator・Howevey讐COuldnotidentifythe COmPOnentOfthephotolnltlatOr.. 如/.P砂∫.30(1991)L1998.. 2・C・J・Whitters,J・M・GirkinandJ.J.Carey,qフt.. 上eJJ.24(1999)67.. 3.A.Jimenez−Planas,J.Martin,C.AbalosandR. Llamas,Quintessenceht.39(2008)e74. 4.VHegde,S.JadhavandGB.Aher,J Conserv かe〃7.12(2009)105. 5.K.−H.Chae and GJ.Sun,Bull.Kofean Chem. ∫oc.19(1998)152.. 6・T.SumlyOShi and W Schnabel,Mdk7VmOl. Cカe刑.186(1985)1811.. 7・U・KoIczak,GRist,K.DietlikerandJ.Wirz,J d椚・C毎刑.∫oc.118(1996)6477. 8・K・L・VanLanduyt,J.Snauwaert,J.DeMunck, M・Peumans,Y Ybshida,A.Poitevln,E. Coutinho,K.Suzuki,RLambrechtsandB.Van Meerbeek,BiomateriaLs28(2007)3757. 9.J.LeprlnCe,J.Devaux,T.Mullier,J.Vrevenand GLeloup,qフerDent.35(2010)220.. 10.B.R.T.Price and C.A.Felix,Dent.ルbter25 (2009)899.. 11・K・L.Van Landuyt,A.Mine,J.De Munck,J. Jaecques,M.Peumans,P.Lambrechts and B. VanMeerbeek,JAcWleS.Dent.11(2009)175. 12・K.L.VanLanduyt,J.DeMunck,A.Mine,M.V Cardoso,M.PeumansandB.VanMeerbeek,J βe〃J・鮎∫.89(2010)1045. 13・M・Cadenaro,F・Antoniolli,S・Sauro,F・R・Tby, R.Di Lenarda,C.Pratl,M.Biasotto,L. Contardo andL.Breschi,EurJ OralSci.113 (2005)525.. 5.Conclusions Inthisstudy,thedifEtrenceinthewavelength distributionofcontemporarylight−Curlngunitswas. determined・Furthermore,We COuld clarifythat SOme COmmerCially available dental adhesives. 14.M.GNeumann,C.C.Schmitt,GC.Ferreiraand I・C・Correa,Dent.Mdter22(2006)576. 15・N・IlieandR・Hickel,Dent.MdterJ27(2008) 221.. 16・W・Tbshima,YNomura,N.Tanaka,S.Shibata, 415.

(8) J・P加opoJym・Sci・乃Cわ〃OLVoJ・24′Nb・4′20日. T.Shintani,K.Shirai,H.Urabe,YNahara,H.. Shintani,々n.J ConservDent.47(2004)442. 17.M.Cadenaro,F.Antoniolli,B.Codan,K.Agee, F.R.Tby,E.S.DorlgO,D.H.Pashley and L. Breschi,Dent.Mdter26(2010)288. 18.A.Kameyama,J.Kato,M.Ybshinarl,Y Kotoku,GAkashiandYHirai,J Photqpob)m. ∫C∼.乃Cゐ〃0/.21(2008)31. 19.H.Arikawa,H.Takahashi,T.Kanle,S.Ban, βe〃才.ルbJerJ28(2009)454.. 20.R.Nomoto,J.F.McCabe,K.Nitta and S. Hirano,0あntology97(2009)109. 2lK.L.VanLanduyt,M.VCardoso,J.DeMunck, M.Peumans,A.Mine,P.LambrechtsandB.. 416. VanMeerbeek,Dent.A4dter25(2009)982. 22.H,Shintani,M.Yamaki and T.Inoue,Dent. 几勿Jerl(1985)124. 23.A.Kameyama,H.Hatayama,J.Kato,A. Haruyama,H.1七raoka,Y Takase,M. Ybshinari and M.Tsunoda,Lase7T Mbd Sci. (inpress).DOI:10.1007/slOlO3−011−0896−Z 24.N.Matsuzawa,I.Ikeshima,K.Fttjibayashiand Y Momoi,々〃.J Co〃∫erVかe〃才.47(2004) 253.. 25.K.Tashiro,N.Matsuzawa,T.Ori,T. Yamamoto,K.FttjibayashiandYMomoi,々n. J Co〃∫erVかe〃〆.47(2004)642..

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Table 1. Light-curing units used in this study  Light-curing unit    (Manufacturer)  Mode  Power  density  (mW/cm 2 )  Diameter (mm)  &lt;Quartz-tungsten-halogen&gt;  D-Lux 2000
Table 2.  Adhesives used in this study
Fig. 3. Emission spectra of light-curing units

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