ABSTRACT
A cast or oil- cont aining dent al lut ing agent : effect s
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st r engt h
Juliana dos Reis DERCELI1, Laiza Maria Grassi FAIS2, Lígia Antunes Pereira PINELLI2
1- Department of Restorative Dentistry, Ribeirão Preto School of Dentistry, University of São Paulo, Ribeirão Preto, SP, Brazil.
2- Department of Dental Materials and Prosthodontics, Araraquara Dental School, Univ. Estadual Paulista - UNESP, Araraquara, SP, Brazil.
Corresponding address: Lígia Antunes Pereira Pinelli - Rua Humaitá, 1680 - Centro - Araraquara - SP - Brazil - 14801-903
- Phone: +55 (16) 3301-6413 - Fax: +55 (16) 3301-6406 - e-mail: [email protected]
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avorable r esult s in t he use of cast or oil polyur et hane ( COP) as pulp capping, m em brane m at er ial, sealer, m out hwash and in bone r epair, associat ed w it h t he fact t hat Ricinuscom m unis is not derived from pet roleum and it is abundant in Brazil, encourage researches LQWKHGHYHORSPHQWRIOXWLQJDJHQWV2EMHFWLYHV7KLVVWXG\FRPSDUHGWKHÀH[XUDOVWUHQJWK
( FS) of a cast or oil- cont aining dent al lut ing agent w it h a w eight per cent age of 10% ( w t % ) of calcium car bonat e ( COP10) w it h RelyX ARC ( RX) aft er m echanical cycling ( MC) and dist illed wat er st orage. Mat er ial and Met hods: Sixt y- four specim ens ( 25x2x2 m m ) w er e fabr icat ed and divided int o t w o gr oups, COP10 and RX ( cont r ol) . Each gr oup was divided int o 4 subgr oups ( n= 8) accor ding t o t he st orage t im e, 24 hour s ( 24 h) or 60 days ( 60 d) , and t he per for m ance ( MC+ FS) or not ( only FS) of t he m echanical cycling t est . The FS ( 10 kN; 0.5 m m / m in) and MC t est s ( 10,000 cycles, 5 Hz, 0.5 m m / m in) w er e car r ied out using an MTS- 810 m achine. The dat a w er e analyzed using ANOVA (α= 0.05) . Result s: The
obt ained FS ( MPa) values w er e: COP10 24h- 19.04± 2.41; COP10 60d- 17.92± 3.54; RX 24h- 75.19± 3.43; RX 60d- 88.77± 6.89. All t he RX specim ens subm it t ed t o MC fract ur ed, w hile t he values for COP10 aft er MC w er e as follow s: COP10 24h- 17.90± 1.87 and COP10 60d- 18.60± 1.60. Conclusions: A cast or oil- cont aining dent al lut ing agent w it h a w eight per cent age of 10% ( w t % ) of calcium car bonat e is r esist ant t o m echanical cycling w it hout
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Ke y w or ds: Biocom pat ible m at er ials. Polyur et hanes. Dent al cem ent s. Mat er ial r esist ance.
Aging.
I N TROD UCTI ON
Polym er s ar e biocom pat ible m at er ials of nat ural or synt het ic origin t hat can be prepared by different m et h od s3 4. I n d en t ist r y, v ar iou s p oly m er s ar e
used, such as silicone, m et hyl m et hacr ylat e and polyur et hane. Cur r ent ly, veget able- polyur et hane, which com bines t he versat ilit y of polym er form ulat ion w h i l e ad d r essi n g t h e g l o b al co n cer n t o w ar d s p r o d u ci n g n ew b i o m at er i al s f r o m su st ai n ab l e r esour ces, has becom e one of t he m ost st udied biom at er ials3. The use of veget able- polyur et hane
der ived fr om cast or oil ( COP) in t he healt h science f i el d s h as b een st u d i ed , an d COP h as sh o w n
fav or able r esu lt s in t est s for biocom pat ibilit y2 2.
Cast or oil is a new m at erial t hat is globally available, and it has r eceived m uch at t ent ion in r ecent year s because of it s availabilit y on a lar ge com m er cial scale23.
Th e COP is a b iocom p at ib le, an t im icr ob ial, ost eoint egrable and absor bable, ost eoconduct ive and ost eoinduct ive13. I n dent ist r y, t he use of t his
polym er has been st udied in dir ect pulp capping5,
as a m em br an e m at er ial2 2, as a sealer3 1, as a
m out hwash28, as bone pr ost hesis and in alveolar
h ealin g7 an d b on e r econ st r u ct ion2 0. I n clin ical
good biocom pat ibilit y for use bot h in soft and har d t issue, has ost eoinduct ive pr oper t ies, and can be bact er icidal and fungicidal w hen com bined w it h calcium car bonat e.
The ver sat ilit y of t he polyur et hane der ived fr om cast or oil as w ell as t he afor em ent ioned posit ive aspect s suppor t t he st udy of COP as a dent al lut ing agent . Alt hough a wide range of dent al lut ing agent s is com m er cially available, t he select ion of a lut ing agent t o be used for a given r est orat ion should not be an ar bit rar y choice. I t m ust be based on a basic know ledge of t he m at er ials available, t he t ype of r est orat ion t o be placed, and t he r equir em ent s
GH¿QHGE\WKHSDWLHQW17 based on t he funct ional and
biological needs2 of a par t icular clinical sit uat ion,
including handling charact er ist ics such as w or king t im e, set t ing t im e, consist ency and ease of rem oval of ex cess m at er ial3 3. As su ch , n o sin gle den t al
lut ing agent is consider ed ideal, and new pr oduct s should be st udied. I t is im por t ant t o charact er ize t he m echanical, physical and biological propert ies of COP. When com par ed w it h zinc phosphat e cem ent , t he COP, w it h t he addit ion of calcium car bonat e, pr esent ed bet t er diam et ral t ensile st r engt h values
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The addit ion of calcium car bonat e is r esponsible for confer r ing radiopacit y t o COP29. Mor eover, t his
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ion exchange at t he bone/ r esin m at r ix int er face15,
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m ar gins. The COP dent al lut ing agent s ar e deem ed st r ong enough t o r esist m ast icat or y st r esses and pr ovide r et ent ion sim ilar t o t hat of zinc phosphat e cem ent , a per m anent cem ent at ion m at er ial29.
I n t he oral cavit y, t he chew ing for ces applied t o r est orat ive m at er ials r esult in cycles of m echanical i m p u l se s t h a t l e a d t o m a t e r i a l f a t i g u e a n d , co n se q u e n t l y, f r a ct u r e . Th e se i m p u l se s ca n b e sim u lat ed in t h e lab or at or y b y p er f or m in g m e c h a n i c a l c y c l i n g , w h i c h a p p r o a c h e s t h e physiological condit ions generat ed by t he chew ing cycle24. Fixed par t ial dent ur es ar e m or e likely t o be
subj ect ed t o bending for ces t han t o ot her t ypes of st r ess10,25,26$VVXFKWKHÀH[XUDOSURSHUWLHVRIWKH
r est orat ive m at er ial ar e m or e im por t ant t han t heir t ensile, shear and com pressive st rengt hs. Moreover,
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appr opr iat e for sim ulat ing t he clinical sit uat ion of m at er ial fat igue4,32 because t he concent rat ion of
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in t he dent al lut ing agent pr ior t o t he fract ur e or displacem en t of t h e r est or at ion m at er ial1 1. Th e
m echanical pr oper t ies of r esinous m at er ials ar e direct ly relat ed t o t he quant it y and t ype of inorganic par t icles8, degr ee of cur e and per cent age of
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Most cur r ent in vit r o st udies include cycling t est ing
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of st r ess on t he m at er ial16,21.
The aim of t his st udy was t o assess t he behavior of COP u n der m ast icat or y st r ess sim u lat ed by
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w it h a w eight per cent age of 10% ( w t % ) of calcium car b on at e w as an aly zed w it h an d w it h ou t t h e per for m ance of t he m echanical cycling t est as w ell as w it h st orage in dist illed wat er. The r esult s w er e com par ed w it h t he r esult s for RelyX ARC. The null hypot hesis was t hat t her e is no differ ence bet w een
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ARC.
M ATERI AL AN D M ETH OD S
The pr ocedur e of t he st udy is sum m ar ized in Figur e 1. For t he COP10 gr oup, 32 specim ens w er e fabr icat ed w it h t h e cast or oil- con t ain in g den t al lut ing agent ( Cast or Oil Polyuret hane - COP, Poliquil Araraquara, Chem ical Polym ers Lt d, Araraquara, SP, Brazil) w it h a w eight per cent age of 10% ( w t % ) of calcium car bonat e ( CaCO3) . For t he cont r ol gr oup, nam ed RX, 32 specim ens w er e fabr icat ed w it h t he r esin cem ent RelyX ARC ( 3M ESPE, Sum ar é, SP, Brazil) . Each gr oup was random ly divided int o 4 subgr oups ( n= 8) accor ding t o t he st orage t im e in dist illed wat er, 24 hour s ( 24 h) or 60 days ( 60 d) , and t he per for m ance or not of t he m echanical cycling ( MC) t est .
The COP was pr ovided in a sachet cont aining polyol, pr epoly m er and calcium car bonat e6. This
poly u r et h an e h as t h e f ollow in g h igh ly r eact iv e gr oups in t he r icinoleic acid st r uct ur e: a car bonyl g r ou p on t h e f ir st car b on , a d ou b le b on d ( or unsat urat ion) on t he nint h car bon and a hydr oxyl gr oup on t he t w elft h car bon. This com binat ion of a hydroxyl group and unsat urat ion occurs exclusively i n t h e ca st o r o i l m o l ecu l e1 4. Pr ep o l y m er w a s
synt hesized fr om m et hylene diphenyl diisocyanat e ( MDI ) and was prepolym erized wit h t he polyol while pr eser v ing 20% of fr ee isocyanat e. When t hese t w o com ponent s w er e m ixed, t he m oist ur e- cur ing k in et ics w as det er m in ed by t h e poly m er izat ion r eact ion b et w een t h e isocy an at e an d h y d r ox y l groups. The st oichiom et ric rat io bet ween t he polyol and t he pr epolym er was equal t o 1: 0.66.
For t he COP1 0 specim ens, t he m at er ial w as m anually m ixed in t he sachet for 2 m inut es. I t was
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This apparat us was placed in a m echanical pr ess under const ant load and st or ed in sat urat ed wat er vapor in a cont ainer lined w it h w et paper at 37° C for one hour9.
accor ding t o t he inst r uct ions of t he m anufact ur er,
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cur ed w it h light at t hr ee point s along it s lengt h on bot h sides for 40 seconds each10. The m at r ix was
placed in a m echanical pr ess under const ant load and st or ed in sat urat ed wat er vapor in a cont ainer lined w it h w et paper at 37° C for one hour9.
Aft er t he init ial st orage per iod of 1 hour, all t he sam ples w er e r em oved fr om t he m at r ix and polished w it h 200 gr it silicon car bide sandpaper ( 3M ESPE) . Then, t hey w er e m easur ed at t hr ee point s using a digit al caliper ( 500- 144B, Mit ut oyo Sul Am er ica Lt d, Suzano, SP, Brazil) t o ver ify t he w idt h and t hickness. A var iance of ± 0.2 m m was accept ed. The sam ples w er e im m er sed in dist illed
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t o t he subgr oups.
All sam ples w er e subj ect ed t o 3- point bending
t est , w hich was conduct ed in a univer sal t est ing m achine ( MTS 810, Mat er ial Test Sy st em , Eden Prairie, MN) equipped wit h t he Test Work 4 soft ware, at a cr osshead of 0.5 m m / m in18 and w it h a 10 kN
load cell. The FS values w er e calculat ed in MPa
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point , I = dist ance bet w een t he suppor t s, b= w idt h of t he sam ples, d= t hickness of t he sam ples) . The MC pr ocedur e w as car r ied out under condit ions equivalent t o t hose used for t he FS t est . Sam ples w er e subm it t ed t o 10,000 cycles at a fr equency of 5 Hz and a cross- head displacem ent of 0.5 m m . The init ial load was 60% of t he m ean FS value previously obt ained. Aft er com plet ing t he MC, sam ples w er e subm it t ed t o FS. Nor m alit y dist r ibut ion w it hin each sam ple was done using Kolm ogor ov- Sm ir nov t est , an d t h e com par ison bet w een t h e ex per im en t al
COP10 RX
24 hours 60 days 24 hours 60 days
Without mechanical cycling
19.04±2.41a 17.92±3.54a 75.19±3.43b 88.77±6.89c
With mechanical cycling
17.90±1.87a 18.60±1.60a * *
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performance of mechanical cycling test
* Specimens did not resist the mechanical cycling
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su b g r o u p s w a s p e r f o r m e d u si n g a n a l y si s o f
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5% (α= 0.05) .
RESULTS
The FS values ar e show n in Table 1. The COP10 specim ens had m ean only about 25% of t he RelyX ARC. The RX sam ples did not r esist t he m echanical cycling and fract ured before t he 10,000 cycles were com plet ed. Tw o- way ANOVA am ong t he subgr oups
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t he FS values as a funct ion of eit her t he “ m echanical cycling” ( F1,28= 0.068; p= .0795) or “ st orage t im e”
( F1,28 S 2QHZD\$129$LGHQWL¿HG
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of RelyX ARC st orage ( F1,14= 24.860, p< .0002) ; it
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st r engt h of t he RX sam ples ( Table 1) .
D I SCUSSI ON
I n t his st udy, t he null hypot hesis was r ej ect ed
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different from t hat of t he RelyX ARC, a com m ercially available and m ost w idely used r esin cem ent . Tw o clinical sit uat ions w er e assessed using condit ions designed t o sim ulat e t he oral envir onm ent : aging was sim ulat ed by st orage in aqueous m edium12,
and chew ing for ces w er e sim ulat ed by m echanical cycling24 7KH FDOFLXP FDUERQDWH ¿OOHU ZDV XVHG
because pr ev ious st udies have show n it s abilit y t o pr ovide radiopacit y t o t he COP and t o supply bact ericidal and fungicidal propert ies t o t he cem ent , propert ies t hat can be a key fact or in t he select ion of a dent al lut ing agent . The addit ion of 10% calcium carbonat e showed good result s regarding diam et ral
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The m echanical propert ies of resinous m at erials ar e d i r ect l y r el at ed t o t h e q u an t i t y an d t y p e ( com posit ion, shape, size and dist r ibut ion) of t he inor ganic par t icles8, degr ee of cur e and per cent age
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par t icles30. The r esult s of t his st udy show ed t hat ,
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COP10 gr oup was low er t han t hat of t he RelyX ARC gr oup. This r esult can be explained by differ ences
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cem ent s.
The RelyX ARC is com posed of t he follow ing: 1 ) an or gan ic m at r ix com posed of m on om er s, p oly m er izat ion in h ib it or s, color m od if ier s an d an init iat or / act ivat or sy st em ; 2) a zir conia/ silica
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3) or gano- silane as a bonding agent bet w een t he
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is com posed of t he follow ing: 1 ) a m at r ix t hat
r esult s fr om t he polym er izat ion of polyest er fr om veget able polyol wit h linear aliphat ic diisocyanat es; 2) 10% ( w t % ) of calcium car bonat e by w eight as
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of a b on d in g ag en t , w h ich cou ld r esu lt in t h e consequent failure in t he linking- up of t he inorganic par t icles w it h t he r esin m at r ix , could be a k ey
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How ever, even t hough t he FS m ean for COP10 was only about 25% of t hat of RelyX ARC, t he FS values w er e sim ilar or slight ly less t han t hose found for lut ing agent s such as zinc phosphat e ( 18 MPa) , glass ion om er cem en t ( 1 5 3 6 MPa) an d r esin
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The specim ens m ade fr om t he r esin cem ent RelyX ARC did not achieve t he FS values r epor t ed
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( 8 6 ± 6 – 1 5 5 ± 7 MPa) in 2 4 h ou r s1 8. How ev er,
aft er 6 0 day s of st orage in dist illed w at er, t his dent al lut ing agent show ed an 18% incr ease in FS in com par ison w it h t he values obt ained aft er 2 4 h ou r s. I t h as b een sh ow n in t h e lit er at u r e t hat m echanical r esist ance r esult s can var y as a
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cur e and t est ing m et hod used12. Accor ding som e
aut hors10,12,26, increases in FS, even in t he presence
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or cont inued polym erizat ion t hat m ay occur in dual-cur e cem ent s.
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st r e n g t h o f t h e COP1 0 sp e ci m e n s r e m a i n e d st at ist ically sim ilar t o t h at ob ser v ed af t er 2 4 hour s of st orage. Accor ding t o t he m anufact ur es of t he COP, aft er 1 hour, t he cem ent has acquir ed st r en g t h , alt h ou g h it can con t in u e t o p r esen t r esidual poly m er izat ion for up t o 36 hour s aft er t he init ial m ixing, t hought m ost of t he isocyanat e-hy dr ox y l r eact ion is com plet ed in 24 hour s. As such, in t his st udy, t he r esidual poly m er izat ion t hat occur r ed bet w een 24 and 36 hour s of st orage
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values. Mor eover, consider ing t hat t he specim ens w er e im m er sed in dist illed w at er an d t h at t h e f r ee isocy an at es m ay h av e r eact ed w it h w at er m olecules, it w as int er est ing t hat t her e w as no decr ease in FS, i.e., t he long- t er m effect of wat er st orage did not affect t he FS of t he COP10, sim ilarly
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deionized wat er31.
The r esult s of t he MC t est show t hat t he RelyX
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m ay be t he r esult of t he lar ge am ount of zir conia/ si l i ca f i l l er ( 6 7 . 5 w t % ) i n co r p o r at ed i n t o t h e m at r ix177KLVDPRXQWRI¿OOHUPD\KDYHLQÀXHQFHG
show ed no change in FS aft er m echanical cycling, possibly due t o t he higher elast icit y provided by t he
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failur e pot ent ial of a cem ent ed r est orat ion under forces is relat ed t o t he m echanical propert ies of t he individual part s ( periodont al ligam ent , t oot h, lut ing agent and rest orat ion)32. Despit e report s of success
of RelyX ARC1,27, cur r ent lit erat ur e show s t hat t he
com par ison s based on adh esiv e pr oper t ies an d
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part ial dent ures ( FPD) cem ent ed wit h RelyX ARC are st ill lim it ed. Then, t his in vit ro st udy was carried out as a pr elim inar y st udy t o invest igat e and com par e t he behavior of t he COP10 under t ension, w it hout
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and fat igue) behavior of cr ow ns or FPD cem ent ed w it h t hese t w o m at er ials in or der t o enhance t he know ledge about COP10 and RelyX ARC.
Despit e t he lim it at ions inher ent t o an in vit r o st udy as w ell as t he low er FS values of t he COP10 t hat w er e obser ved, t his dent al lut ing agent can st ill be consider ed a pr om ising m at er ial due t o i t s ch ar act er i st i cs r el at ed t o b i o co m p at i b i l i t y, elast icit y, m ech an ical st r en g t h an d v er sat ilit y
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Mor eover, Ricinus com m unis is a plant easily found in Brazil wit h great pot ent ial in t he m anufact uring of product s derived from it s oil. As such, fut ure st udies sh ou ld be con du ct ed t o assess COP con t ain in g higher concent rat ions of CaCO3 and t he addit ion
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im pr ove it s m echanical r esist ance, causing it t o have pr oper t ies sim ilar t o t hose of com m er cially available r esin cem ent s.
CON CLUSI ON
A cast or oil- cont aining dent al lut ing agent wit h a 10% weight percent age ( wt % ) of calcium carbonat e r esist ed m echanical cycling w it hout decr eases in
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ACKN OW LED GEM EN TS
The aut hors t hank São Paulo Research Foundat ion
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2006/ 02821- 8) .
REFEREN CES
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