Ftir and nmr of hydroxyapatit

FTIR and NMR of Hydroxyapatite incorporation with Heat Cured Acrylic

Amer A. Taqa Nadira A .Zena J.

University of Mosul, College of Dentistry

Acrylic Resin Denture Base Material History

In 1937, poly methylmethacrylate (PMMA) was In 1937, poly methylmethacrylate (PMMA) was introduced and used widely as a denture base introduced and used widely as a denture base material. PMMA provided enhanced physical material. PMMA provided enhanced physical and esthetic properties; in addition, it was and esthetic properties; in addition, it was readily available, inexpensive and relatively readily available, inexpensive and relatively eases of use, and reliance on simple processing eases of use, and reliance on simple processing equipment (Nejatian et al., 2006).equipment (Nejatian et al., 2006).

REVEW OF LITERATURE :

The hydroxyapatite (CaThe hydroxyapatite (Ca1010(PO(PO44))66(OH)(OH)22) has ) has been widely used as a bone substitute, been widely used as a bone substitute, taking into account its biocompatibility, taking into account its biocompatibility, as its mineral components are similar to as its mineral components are similar to those of the bones and teeth of the those of the bones and teeth of the human body. Synthetic hydroxyapatite is human body. Synthetic hydroxyapatite is an important biomaterial used in many an important biomaterial used in many medicine applications in bulk, as a medicine applications in bulk, as a coating, or as a component of a coating, or as a component of a composite .composite .

Pure Hydroxyapatite powder is white. Pure Hydroxyapatite powder is white. Naturally occurring apatites can, however, Naturally occurring apatites can, however, also have brown, yellow, or green also have brown, yellow, or green colorations, comparable to the colorations, comparable to the discolorations of discolorations of dental fluorosis. Up to . Up to 50% of 50% of bone is made up of a modified form is made up of a modified form of the inorganic mineral Hydroxyapatite of the inorganic mineral Hydroxyapatite known as known as bone mineral (Junqueira (Junqueira et alet al., ., 2003).2003).

Hydroxyapatite (HA) :

REVEW OF LITERATURE

ReliningRelining

Relining is the process of Relining is the process of adding some materials to the adding some materials to the tissue side of denture to fill tissue side of denture to fill the space between the tissue the space between the tissue and the denture base ( Robert, and the denture base ( Robert, 1985; Levin and Richared, 1985; Levin and Richared, 2002).2002).

Aims of Study:

1.1. incorporation of synthetic Hydroxyapatite incorporation of synthetic Hydroxyapatite

(2%,5%) extracted from eggshells then study (2%,5%) extracted from eggshells then study

FTIR, HNMR spectra of heat cured acrylic FTIR, HNMR spectra of heat cured acrylic

resin denture base mixed or relined denture resin denture base mixed or relined denture

base.base.

2.2. Biocompatibility of denture synthetic Biocompatibility of denture synthetic

Hydroxyapatite on rabbits.Hydroxyapatite on rabbits.

3.3. Other physical and mechanical properties Other physical and mechanical properties

also study.also study.

MATERIALS AND METHODSMATERIALS AND METHODS

Materials Used in the preparation samples of this Study

No.MaterialManufacture

1.Dental stone.Elite stone (Zehrmack)/

2.Heat cured acrylic resin.RESPAL NF(RESINA

PALATIA CALDO/Italy)

3.HydroxyapatitePrepared from egg shell

4.Separating medium.Isodent

5.Formaldehyde 3A MEDES company,

6.Hard elastic foils 3mm 2.5mm 1.5mmRotex medica Gmbh

7.Ketamine hydrochloride general anasthesiaTiergesudheit Gmbh

8.Xylazine(sedative analgesic)Horsterweg 26A

9.Absolute Alcohol BDH Company

10Pure vaslineComercial available

Total Samples 171 divided according to the test for each subgroup 5 Samples

5% HA gp2% HA gp Control 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

Samples preparation with and without additive (HA): Polymer and monomer of heat cured acrylic resin Polymer and monomer of heat cured acrylic resin have been mixed in ratio (2.2 gm:1ml by volume), have been mixed in ratio (2.2 gm:1ml by volume), (according to the manufacturer instructions).(according to the manufacturer instructions). While the experimental groups of heat cured acrylic While the experimental groups of heat cured acrylic resin with additive have been prepared by mixing resin with additive have been prepared by mixing powder (polymer) (22gm polymer with 0.5gm powder (polymer) (22gm polymer with 0.5gm hydroxyapatite for 2% and 8.8gm polymer with 0.5gm hydroxyapatite for 2% and 8.8gm polymer with 0.5gm hydroxyapatite for 5%)hydroxyapatite for 5%)

A B

Method

Relining sample preparation:

The samples were prepared by placing hard elastic foil The samples were prepared by placing hard elastic foil with 1.8mm thickness for indentation hardness and with 1.8mm thickness for indentation hardness and residual monomer test, 1.5 mm for transverse strength, residual monomer test, 1.5 mm for transverse strength, dimensional accuracy test and 2mm for water sorption dimensional accuracy test and 2mm for water sorption and solubility test to the desired length and width and solubility test to the desired length and width specified for each test (Hasan, 2002).specified for each test (Hasan, 2002).

Method

Relined part of denture base was prepared Relined part of denture base was prepared mixed with hydroxyapatitemixed with hydroxyapatite

Method

A

B C D

E

F

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

H1NMR spectra was done in H1NMR spectra was done in Chemistry Department, Chemistry Department, Colorado state University, USA Colorado state University, USA using CIF-MR 400-Vnmrs400 in using CIF-MR 400-Vnmrs400 in CDClCDCl33 solvent. solvent.

Biocompatibility test

2mm width

5mm

len

gth

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

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

(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

RESULTSRESULTS

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

and the absorbance peak of and the absorbance peak of the C=O from the ester group the C=O from the ester group appear around 1733 cm-1) appear around 1733 cm-1) and some important bands and some important bands for HA 3446 cm-1 for OH for HA 3446 cm-1 for OH stretching, 992cm-stretching, 992cm-1(V1(V11PO4),601 and 571cm-1 PO4),601 and 571cm-1 for (Vfor (V 4 4 PO PO44) . ) .

Control sample

C=OC=C

Acrylic with 2% HA

C=CC=O

νOH

ν1PO4

ν4PO4

ν4PO4

Arylic with 5% HA

C=CC=O

ν1PO4

ν1PO4

ν4PO4

νOH

The results showed there is The results showed there is now reaction between now reaction between Additive HA (2% and 5%) and Additive HA (2% and 5%) and poly methyl methacrylate poly methyl methacrylate after polymerization also the after polymerization also the HA still incorporated with HA still incorporated with PMMA. PMMA.

1H NMR spectra show two 1H NMR spectra show two highly intense broad peaks highly intense broad peaks centered at 0.7 and 5.6 ppm, centered at 0.7 and 5.6 ppm, respectively. The NMR peak respectively. The NMR peak near 1 ppm is due to hydroxyl near 1 ppm is due to hydroxyl group in HA,(Yesinowski 1987). group in HA,(Yesinowski 1987).

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).

-COOCH3

-CH2-C-

-C-CH3

PMMA

OH of HA

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

OsteocyteBlood vessel

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.

Conclusions:

The present study comes up with the The present study comes up with the following conclusions:following conclusions:

In FTIR and H1NMR spectra In FTIR and H1NMR spectra test showed that the test showed that the addition of 2% and /or 5% addition of 2% and /or 5% hydroxyapatite to heat cured hydroxyapatite to heat cured acrylic resin denture base acrylic resin denture base material resulting a material resulting a homogenous mixture, homogenous mixture, without chemical reaction.without chemical reaction.

Using Hydroxyapatite as Using Hydroxyapatite as additive for denture lining additive for denture lining show biocompatibility of show biocompatibility of the material and enhance the material and enhance new bone formation.new bone formation.