Ftir and nmr of hydroxyapatit


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Ftir and nmr of hydroxyapatit

  1. 1. FTIR and NMR of Hydroxyapatite incorporation with Heat Cured Acrylic Amer A. Taqa Nadira A. Zena J. University of Mosul, College of Dentistry
  2. 2. Acrylic Resin Denture Base Material History In 1937, poly methylmethacrylate (PMMA) was introduced and used widely as a denture base material. PMMA provided enhanced physical and esthetic properties; in addition, it was readily available, inexpensive and relatively eases of use, and reliance on simple processing equipment (Nejatian et al., 2006). REVEW OF LITERATURE :
  3. 3. The hydroxyapatite (Ca10(PO4)6(OH)2) has been widely used as a bone substitute, taking into account its biocompatibility, as its mineral components are similar to those of the bones and teeth of the human body. Synthetic hydroxyapatite is an important biomaterial used in many medicine applications in bulk, as a coating, or as a component of a composite .
  4. 4. Pure Hydroxyapatite powder is white. Naturally occurring apatites can, however, also have brown, yellow, or green colorations, comparable to the discolorations of dental fluorosis. Up to 50% of bone is made up of a modified form of the inorganic mineral Hydroxyapatite known as bone mineral (Junqueira et al., 2003). Hydroxyapatite (HA) : REVEW OF LITERATURE
  5. 5. Relining Relining is the process of adding some materials to the tissue side of denture to fill the space between the tissue and the denture base ( Robert, 1985; Levin and Richared, 2002).
  6. 6. Aims of Study: 1. incorporation of synthetic Hydroxyapatite (2%,5%) extracted from eggshells then study FTIR, HNMR spectra of heat cured acrylic resin denture base mixed or relined denture base. 2. Biocompatibility of denture synthetic Hydroxyapatite on rabbits. 3. Other physical and mechanical properties also study.
  8. 8. Materials Used in the preparation samples of this Study No. Material Manufacture 1. Dental stone. Elite stone (Zehrmack)/ 2. Heat cured acrylic resin. RESPAL NF(RESINA PALATIA CALDO/Italy) 3. Hydroxyapatite Prepared from egg shell 4. Separating medium. Isodent 5. Formaldehyde 3A MEDES company, 6. Hard elastic foils 3mm 2.5mm 1.5mm Rotex medica Gmbh 7. Ketamine hydrochloride general anasthesia Tiergesudheit Gmbh 8. Xylazine(sedative analgesic) Horsterweg 26A 9. Absolute Alcohol BDH Company 10 Pure vasline Comercial available
  9. 9. Total Samples 171 divided according to the test for each subgroup 5 Samples 5% HA gp2% HA gpControl gp HCAR HCAR Relined with HCAR with 5% HA Samples 5% HCAR mixed 5% HA Samples HCAR relined with HCAR With 2% HA Samples HCAR Mixed with2% HA Samples Measurement properties indentation hardness , transverse strength , water sorption and solubility, tensile strength, dimensional accuracy, residual monomer , FTIR , and biocompatibility and microscopical examination of Prepared polymer . HCAR : Heat Cured acrylic resin. HA : Hydroxyapatite
  10. 10. Samples preparation with and without additive (HA): Polymer and monomer of heat cured acrylic resin have been mixed in ratio (2.2 gm:1ml by volume), (according to the manufacturer instructions). While the experimental groups of heat cured acrylic resin with additive have been prepared by mixing powder (polymer) (22gm polymer with 0.5gm hydroxyapatite for 2% and 8.8gm polymer with 0.5gm hydroxyapatite for 5%) A B Method
  11. 11. Relining sample preparation: The samples were prepared by placing hard elastic foil with 1.8mm thickness for indentation hardness and residual monomer test, 1.5 mm for transverse strength, dimensional accuracy test and 2mm for water sorption and solubility test to the desired length and width specified for each test (Hasan, 2002). Method
  12. 12. Relined part of denture base was prepared mixed with hydroxyapatite Method A B C D E F
  13. 13. FTIR Test: Samples prepared with dimension 10x4x4(±0.03)mm (Urban et al., 2007) samples were removed from water and dried in air and then scraped using a sharp, clean and sterile wax knife to obtain powder of the polymerized samples. The FTIR spectra was carried by Tensor 27 FTIR spectrophotometer Method
  14. 14.  H1NMR spectra was done in Chemistry Department, Colorado state University, USA using CIF-MR 400-Vnmrs400 in CDCl3 solvent.
  15. 15. Biocompatibility test 2mm width 5mmlength Four local bred male rabbits, 4-6 months old with an average weight 1.250-1.350 Kg were used and the animals were housed in animal house prepared for this purpose, the animals were diet of vegetables 2 times daily (AL-Saigh, 2007). Method
  16. 16. The anesthetized animal was laid on it is abdomen on the operation board. The fur was shaved in 2 areas of the rabbits mandible one on right side and other on the left Method
  17. 17. (the first rabbit in the right side the control sample is placed and on the left side the 2%hydroxyapetite sample is placed and the second rabbit on the right side the control sample is placed and on left side the 5% hydroxyapetite sample is placed) (Jones et al., 1978). Method
  18. 18. RESULTS
  19. 19. FTIR test : In the IR charts two important absorbance peaks in poly metheylmethacrylate appeared (the absorbance of the C=C band from the methacrylate group which appear around 1683 cm-1
  20. 20.  and the absorbance peak of the C=O from the ester group appear around 1733 cm-1) and some important bands for HA 3446 cm-1 for OH stretching, 992cm-1(V1PO4),601 and 571cm-1 for (V 4 PO4) .
  21. 21. Control sample C=O C=C
  22. 22. Acrylic with 2% HA C=CC=O νOH ν1PO4 ν4PO4 ν4PO4
  23. 23. Arylic with 5% HA C=CC=O ν1PO4 ν1PO4 ν4PO4 νOH
  24. 24.  The results showed there is now reaction between Additive HA (2% and 5%) and poly methyl methacrylate after polymerization also the HA still incorporated with PMMA.
  25. 25.  1H NMR spectra show two highly intense broad peaks centered at 0.7 and 5.6 ppm, respectively. The NMR peak near 1 ppm is due to hydroxyl group in HA,(Yesinowski 1987).
  26. 26. The observed NMR peak around 5.25 ppm indicates surface-adsorbed water in the nanocrystalline of HA. Such kinds of results are well known in the literature for HA (Miquel 1990).
  27. 27. -COOCH3 -CH2-C- -C-CH3 PMMA OH of HA
  28. 28. Biocompatibility Test: Biocompatibility test shown new bone formation in the rabbits after 30 days of implantation for both 2% and 5% Hydroxyapatite samples according to decision of intra examiner specialist of oral pahology A.Controlled bone (without additives) C. new bone in sample with(5%Hydroxyapatite) B. new bone in sample with(2% Hydroxyapatite) Blood vesselOsteocyte Osteocyte Blood vessel
  29. 29. The histopathological examination showed more new bone trabeculae formation in the (HA) than normal bone, a finding that agrees with earlier study ( AL-Khafaji, 2001) which showed active bone formation started after one month of implantation. This finding may be due to more late neovascularization and release of calcium from the graft into surrounding tissue.
  30. 30. Conclusions: The present study comes up with the following conclusions:
  31. 31.  In FTIR and H1NMR spectra test showed that the addition of 2% and /or 5% hydroxyapatite to heat cured acrylic resin denture base material resulting a homogenous mixture, without chemical reaction.
  32. 32.  Using Hydroxyapatite as additive for denture lining show biocompatibility of the material and enhance new bone formation.