Characterization and analyses of acid- extractable and leached trace elements in dental cements

J. Camilleri et al, International Endodontic Journal 2012

Presenter: PGY1

Outline
Introduction Materials and Methods Results and Discussion Conclusion

Introduction

Ideal Root-end Filling Material

Well tolerated by periapical tissues Adhere to the tooth structure Resistant to dissolution Promote cementogenesis Bacteriocidal to bacteriostatic Noncorrosive Not stain tooth or periradicular tissue Readily available and easy to handle Allow adequate working time, then set quickly Radiopaque (medicolegal reasons)
Grossman L: Endodontic practice, ed 7, Philadelphia, 1970, Lea & Febiger

Ideal Root-end Filling Material

Hydraulic nature: set and develop their properties in a wet environment

Interest in the use of Portland cement as a root-end filling material

MTA
MTA= Portland cement + bismuth oxide Bismuth oxide is added as a radiopacifier Desirable physical and mechanical properties
Torabinejad et al. 1995, Islam et al. 2006, Camilleri 2008a, 2010, Nekoofar et al. 2010

Bioactive when in contact with tissue fluids

MTA v.s. Portland cement

The presence of bismuth oxide in MTA
Torabinejad & White 1995

The fineness of MTA

Dammaschke et al. 2005

The lower levels of calcium aluminate and calcium sulphate in MTA

Harmful Trace Elements

Arsenic (As)
Arsenic poisoning, leading to multiple organ failure and death

Lead (Pb)
A neurotoxin that accumulates both in soft tissues and the bones, damaging the nervous system and causing brain disorders

Chromium (Cr)
Toxic, mutagenic and cariogenic, allergic reaction

Harmful Trace Elements

Traces of arsenic, lead and chromium have been reported in both grey and white MTA
Duarte et al. 2005, Monteiro Bramante et al. 2008, De-Deus et al. 2009, Chang et al. 2010, Matsunaga et al. 2010, Schembri et al. 2010

Raising concern: MTA is applied in contact with both hard and soft human tissues

New Materials
Laboratory-grade raw materials: pure tricalcium silicate, produced in a laboratory using the solgel method Chun-Cheng et al. 2009
Good bioactivity Induce apatite formation in the presence of simulated body fluid Zhao et al. 2005, Chun-Cheng et al. 2009 Products available Biodentine (Septodont, Saint-Maur-des-Fosses, France) Bioaggregate (Innovative Bioceramix Inc. VerioDental, Vancouver,
Canada)

Aim
Determination of the elemental constitution and investigation of the total and leachable arsenic, chromium and lead in
Portland cement Pure tricalcium silicate mineral trioxide aggregate (MTA) Angelus Biodentine Bioaggregate

Materials and Methods

 Materials Characterization of cements

Determination of acid-soluble ion Cr, As and Pb content Determination of Cr, As and Pb ion release in physiological solution

Materials
White Portland cement MTA Angelus Tricalcium silicate Biodentin Bioaggregate

White Portland cement

Content
Tricalcium silicate (CaO)3 SiO2 Dicalcium silicate (CaO)2 SiO2 Tricalcium aluminate (CaO)3 Al2O3 Tetracalcium aluminoferrite (CaO)4 Al2O3 Fe2O3 Gypsum CaSO4 2 H2O

Mass %
4575% 732% 013% 018% 210%

More expensive than the gray product Water/Cement ratio 0.30

MTA Angelus
White portland cement 80% + Bismuth oxide 20% Water/Cement ratio 0.35

Tricalcium silicate
(CaO)3 SiO2 Water/Cement ratio 0.35

Biodentin
Powder: tricalcium silicate, dicalcium silicate
Zirconium oxide as a radiopacifier Calcium carbonate is incorporated for both its biocompatibility and its calcium content

Liquid: calcium chloride and a hydrosoluble polymer

The hydrosoluble polymer is based on polycarboxylate Calcium chloride and fine particle sizes: Rate of the setting time

Bioaggregate
Main: calcium silicate oxide (Ca3(SiO4)O or Ca3SiO5) and calcium silicate Others: hydroxyapatite, calcium phosphate silicate, calcite Tantalum oxide as a radiopacifier. Bioaggregate is free of calcium aluminate
Park e al. 2010

X-ray fluorescence
Chemical analysis of the cement powders and the liquids available for mixing Biodentine and Bioaggregate (Bio A)
Liquid: Prolene film Powders: Mylar film

Determination of acid-soluble ion Cr, As and Pb content

The total trace metal was determined using the ISO 9917-1 (2007) method
3g powder

liquid

Placed in a plastic bag

Care in an incubator at 37 and 100% humidity for 24h

 2g powder placed in [HCL]=2.4 mol/L, 50 ml Slurry swirled, lightly stoppered and allowed to stand for 16 h

crushed to a very fine powder

Supernatant transferred to a stoppered acid-washed plastic tube Arsenic, lead and chromium content measured

Inductively Coupled PlasmaMass Spectrometer

Centrifuged in a tube for 10 min

Determination of Cr, As and Pb ion release in physiological solution

2 mm Materials cured for 24 h at 37 and 100% humidity

15 mm

Materials placed in 10 mL Hanks balanced salt solution for 28 days in an incubator at 37

Results and Discussion

Characterization of unhydrated cements

MTA Angelus
Both MTA Angelus and Portland cement exhibited similar constituents, and both had an aluminate phase The MTA Angelus did not contain sulphate
Indicating the low to negligible presence of gypsum in the cement Gypsum reduce the setting time MTA Angelus setting time: 1015 min
Santos et al. 2008, Vivan et al. 2009

MTA Angelus
MTA Angelus: 10.5% inclusion of bismuth oxide
20% loading reported in the MTA patent
Torabinejad and White 1995

Same can be said for ProRoot MTA

Camilleri 2008b, Belo-Reyes et al. 2009

Reduced radiopacity of MTA Angelus

Camilleri & Gandolfi 2010

Tricalcium Silicate Cement, Biodentine and Bioaggregate

The tricalcium silicate cement, Biodentine and Bioaggregate had a similar chemical composition All lacked the tricalcium aluminate phase as claimed by the manufacturers and verified by others
Park et al. 2010

Risk of Alzheimers when Aluminum come in close contact with human tissues
Forbes & Gentleman 1998

Biodentine and BioAggregate

Biodentine
Biodentine liquid incorporated a chloride
Added Portland cement to accelerate the setting reaction thus shorten the setting time
Nagataki 1995

Addition of calcium chloride to Portland cement and mineral trioxide aggregate marked reduction in the setting time of the cement demonstrated
Ber et al. 2007, Wiltbank et al. 2007, Bortoluzzi et al. 2009

Determination of acid-soluble Cr, As and Pb content

Trace Element Contamination: Acid

The ISO recommendation for maximum total arsenic content in dental materials is set at 2 mg kg-1 ISO 9917-1 (2007)
Levels of acid-extractable arsenic below the ISO limit in previous studies (Monteiro Bramante et al. 2008) but high in later (Schembri et al. 2010) and current studies Short time for the acid to be in contact with the cement Solution should be allowed to stand for 16h

Trace Element Contamination: Acid

The data are expressed in ppm in other publications
De-Deus et al. 2009, Chang et al. 2011

Not taking into consideration the sample weight and volume of the solution used for the extraction Such data cannot be compared to levels of contamination recommended by ISO standards

Trace Element Contamination: Acid

In the present study, all the materials tested had higher levels of arsenic than the limit set by ISO 9917-1 (2007)
High concentrations of acids and the quantity of dissolved solid content Nonspecific matrix effects

Determination of Cr, As and Pb release in physiological solution

Trace Element Contamination: HBSS

Levels of arsenic leached in water for biomaterials based on Portland cement were reported to be low and below what is considered to be harmful
Duarte et al. 2005

In the current study

All had very low levels of trace element contamination when compared to Portland cement These materials should be considered safe to use No set limits for leachable trace elements in dental standards

Conclusion

 Dental materials based on tricalcium silicate cement and MTA Angelus release minimal quantities of trace elements when in contact with simulated body fluids This indicates that the dental materials investigated in this study are safe for clinical use The results of acid extraction could be affected by nonspecific matrix effects by the cement

Thanks for your attention!

Presenter: R1