KR20040005200A - Multifunctional dental alginate impression material - Google Patents

Abstract

PURPOSE: Provided is a multi-functional dental alginate impression material composition which involves excellent fluoride discharge and antimicrobial effects. CONSTITUTION: A multi-functional dental alginate impression material composition comprises: 100wt.% of powdery impression material; and 0.5-2.5wt.% of sodium fluoride, 0.5-1.5wt.% of stannous fluoride and 1-2.5wt.% of water-soluble chitosan powder, based on the weight of the powdery impression material. The powdery impression material comprises sodium alginate, calcium sulfate, diatomaceous earth, borax, magnesium oxide, potassium chloride, sodium acetate, sodium phosphate, and zinc fluoride.

Description

Multifunctional dental alginate impression material

The present invention relates to a multifunctional dental alginate impression material, and more particularly, dental alginate impression material powder obtained by adding a fluorine compound such as sodium fluoride and fluorite and additionally water-soluble and partially water-soluble chitosan to the dental alginate impression material powder. And a method for producing the same.

Dental alginate impression materials are known to have lower accuracy, detail reproduction, and tear strength than dental rubber impression materials, but they are easy to use, have some precision, and moisture Even if there are advantages such as not causing an inaccurate hike, if the above disadvantages are compensated to some extent, much demand can be expected.

Mac Pherson et al. Reported the difference in compressive strength and characteristics according to the curing time of alginate impression materials [Mac Pherson GW, Craig RG, Peyton FA: Mechanical properties of hydrocolloid and rubber impression materials. J. Dent. Res ., 46: 714-721, 1967], and recent studies on micropart reproducibility and affinity with gypsum [Owen CP: An investigation into the compatibility of some irreversible hydrocolloid impression materials and dental gypsum products. Part I. Capacity to record grooves on the international standard die. J. Oral. Rehabil ., 13: 93-103, 1986; Owen CP: An investigation into the compatibility of some irreversible hydrocolloid impression materials and dental gypsum products. Part II. A refined discriminatory procedure. J. Oral Rehabil ., 13: 147-162, 1986; Reisbick MH, Johnston WM, Rashid RG: Irreversible hydrocolloid and gypsum interactions. Int. J. Prosthodont ., 10: 7-13, 1997].

Although there is much debate about the safety of fluoride materials used in dentistry, it has been found that the addition of fluorine as an ingredient of the alginate impression material has the advantage of promoting the hardening of gypsum model material to improve the surface condition of the model [Buchan S, Peggie RW: Role of ingredients in alginate impression compounds. J. Dent. Res ., 45: 1120-1129, 1966. As a result, some of the commercially available dental alginate impression materials contain fluorine. Hattab notes that the fluoride content of 10 alginate impression material powders is about 0.44 to 2.42% [Hattab F: Absorption of fluoride following inhalation and ingestion of alginate impression materials. Pharmacol. Ther. Dent ., 6: 79-86, 1981. Hattab also found that the fluoride-added alginate impression material was contacted with enamel partially demineralized for 4 minutes and evaluated for inhibition of enamel demineralization. on the acid resistance of demineralized human enamel. Acta. Odontol. Scand ., 42: 175-181, 1984].

In addition, Anastassiadou et al. Demonstrated that surface reproducibility is superior as the pH nears alkaline during hardening of alginate impression materials. [Anastassiadou V, Dolopoulou V, Kaloyannides A: Relationship between pH changes and dimensional stability in irreversible hydrocolloid impression material during setting. Int. J. Prosthodont ., 8: 535 to 540, 1995], and reports on biocompatibility Sydiskis and Gerhardt reported some degree of cytotoxicity after evaluating the cytotoxicity of commercial alginate impression materials [Sydiskis RJ, Gerhardt DE: Cytotoxicity of impression materials. J. Prosthet. Dent ., 69: 431-435, 1993.

On the other hand, as the research on chitosan has been actively conducted recently, many researches on the application method in the dentistry field have been reported. Sano et al. Found that the chitosan solution significantly reduced the amount of plaque and inhibited attachment of plaque in antimicrobial activity against oral microorganisms [Sano H, Shibasaki K, Matsukubo T, Takaesu Y: Comparison of the activity of four chitosan derivatives in reducing initial adherence of oral bacteria onto tooth surfaces. Bull. Tokyo Dent. Coll ., 42: 243-249, 2001; Sano H, Shibasaki K, Matsukubo T, Takaesu Y: Effect of rinsing with phosphorylated chitosan on four-day plaque regrowth. Bull. Tokyo Dent. Coll ., 42: 251-256, 2001].

Thus, the inventors of the present invention was prepared by adding a certain amount of sodium fluoride and fluorite to the conventional dental alginate impression material to prepare a composition of the multi-functional dental alginate impression material, and further prepared by adding a water-soluble or partially water-soluble chitosan, the obtained impression material composition As a result of measuring the mechanical and biocompatibility of, the result was equivalent to or higher than that of the conventional one. The present invention was completed by finding that the secondary infection and cross-infection of dental workers can be reduced by reducing the number of microorganisms in the dental surface and the gingival epithelium after the acquisition.

It is an object of the present invention to provide a dental alginate impression material composition and a method for manufacturing the same, which are suitable for domestic use conditions and apply fluorine to the tooth surface during the impression acquisition process and exhibit antibacterial effect to prevent cross-infection.

1 is a graph showing a change in pH over time of the alginate impression material powder of the present invention.

Figure 2 is a graph showing the change in viscosity with time of the alginate impression material powder added chitosan of the present invention.

The present invention provides a dental alginate impression material composition that can reduce the infection by applying fluorine to the tooth during the impression acquisition process to increase the anti-cariousness, giving the number of microorganisms of the tooth surface and gingival epithelium after the impression acquisition.

The dental alginate impression material composition according to the present invention is obtained by adding a fluorine compound and chitosan to a known impression material powder.

More specifically, the dental alginate impression material first composition of the present invention is:

Sodium alginate, calcium sulfate, diatomaceous earth, borax, magnesium oxide, potassium chloride, sodium acetate, sodium acetate per 100 parts by weight of the impression material powder containing phosphate) and zinc fluoride,

0.5 to 2.5 parts by weight of sodium fluoride, which is a fluorine compound, and 0.5 to 1.5 parts by weight of fluoride; And

1 to 2.5 parts by weight of a water-soluble or partially water-soluble chitosan powder.

In addition, the second composition of the dental alginate impression material of the present invention:

Sodium alginate, calcium sulfate, diatomaceous earth, borax, magnesium oxide, sodium acetate, sodium phosphate, zinc fluoride Based on 100 parts by weight of the impression material powder containing fluoride and zinc oxide,

0.5 to 2.5 parts by weight of sodium fluoride or 0.5 to 1.5 parts by weight of fluoride; And

1 to 2.5 parts by weight of a water-soluble or partially water-soluble chitosan powder.

Hereinafter, the present invention will be described in more detail.

The evaluation criteria of dental alginate impression material are summarized as follows.

Iii) The powder must be homogeneous and free of impurities.

Ii) be biocompatible when tested by the method of ISO 10993 or ISO 7408.

Iii) The mixture should be homogeneous, not clumped or agglomerated when visually mixed by the method suggested by the manufacturer, and the surface of the impression should be smooth.

V) Mixing time should be within 60 seconds.

Ⅴ) The compatibility with gypsum and reproducibility of micro parts should be cleanly separated from gypsum model made by gypsum recommended by the manufacturer and the model surface should be smooth.

석고) Gypsum model injected into impression should reproduce 50 ㎛ line without any break. 변형) The elastic recovery rate after deformation should be 95% or more and the compressive strain (flexibility) should be 5 ~ 20%.

I) The compressive strength is to be at least 0.35 MPa.

Accordingly, the present invention adopts an impression material powder that satisfies the above conditions, and further contains a fluorine compound and chitosan.

The impression material powder is sodium alginate, calcium sulfate, diatomaceous earth, borax, magnesium oxide, sodium acetate, sodium phosphate and Zinc fluoride and potassium chloride or zinc oxide are optionally included therein, the composition of which is shown in Table 1 below.

Sodium alginate Calcium sulfate Diatomaceous earth borax Magnesium oxide Potassium chloride Sodium acetate Sodium phosphate Zinc fluoride Zinc oxide Powder (Ⅰ) 10.0 to 12.0 10.0 to 12.0 64.0-68.0 1.5 to 2.0 1.5 to 2.0 1.5 to 2.0 1.5 to 2.0 1.8 to 2.2 1.5 to 2.0 - Powder (Ⅱ) 10.0 to 12.0 10.0 to 12.0 64.0-68.0 1.5 to 2.0 1.5 to 2.0 - 1.5 to 2.0 1.8 to 2.2 1.5 to 2.0 1.5 to 2.0

The impression material powders (I) and (II) were in compliance with the specifications in the range of 5 to 20% of flexibility, the elastic recovery rate was similar to the commercial product, and the curing time was also similar to the commercial product at 1.5 to 5 minutes. In addition, although the compressive strength was in conformity with the specification defined as 0.35 MPa or more, the reproducibility of the micro parts was different depending on the blending ratio, but all showed the appropriate values in the specification.

More preferably, the (I) impression material powder is:

Sodium alginate 11.35 wt%, calcium sulfate 11.55 wt%, diatomaceous earth 65.6 wt%, borax 1.9 wt%, magnesium oxide 1.9 wt%, potassium chloride 1.9 wt%, sodium acetate 1.9 wt%, sodium phosphate 2.0 wt% and zinc fluoride 1.9 wt% Contains%;

(II) The impression material powder is:

Sodium alginate 11.35 wt%, calcium sulfate 11.55 wt%, diatomaceous earth 65.6 wt%, borax 1.9 wt%, magnesium oxide 1.9 wt%, sodium acetate 1.9 wt%, sodium phosphate 2.0 wt%, zinc fluoride 1.9 wt% and zinc oxide 1.9 wt% Contains%

It was confirmed that the viscosity of sodium alginate in the impression material powder affects the flexibility and elastic recovery of the final dental alginate impression material composition. In the present invention, sodium alginate having a medium viscosity of 300 to 400 cp and high viscosity of 500 to 600 cp. Use

According to a preferred embodiment, when the high viscosity sodium alginate is used, the compressive strain, elasticity, curing time and fluorine emission amount, compressive strength, etc. are slightly superior to those of the medium viscosity, but the overall difference does not appear (Table 3 and Table 4). Reference).

In addition, the impression material powder is a dental impression material having a certain degree of strength and mixing well, the size is limited in order to smooth the surface state, in the present invention was used to crush the sieve to 100 ㎛ or less. Once each composition is uniformly mixed and then adjusted to an appropriate particle size by using a ball mill or the like, it is possible to obtain uniform particles by sieving.

The impression material powder used maintains a neutral pH over time. In order to confirm this, distilled water was mixed with the impression material powder composition (I) and (II) containing sodium alginate having a medium viscosity and a high viscosity, and the pH change was measured over time. It could be confirmed (see FIG. 1). In addition, as a result of using a commercially available product for comparison under the same conditions, the pH was rapidly reduced to 3 to 4 within 5 minutes after mixing to show acidity.

By adding a fluorine compound, which is a second component of the present invention, to the impression material powder, a fluorine coating effect of the impression material is obtained on the teeth in the pulling process, and the surface state is improved.

However, when the excess amount is added, the compressive strain, elastic recovery rate and the like may be slightly lowered, and the content thereof is limited to 0.5 to 2.5 parts by weight based on 100 parts by weight of the impression material powder.

Any fluorine compound that can be used may be any compound that can be used in the art and is not particularly limited in the present invention, but is preferably selected from among sodium fluoride, fluorite and mixtures thereof. At this time, in the case of using sodium fluoride or fluorite, the respective contents will be different in order to obtain desirable physical properties. For the case of sodium fluoride, 0.5 to 2.5 parts by weight and 0.5 to 1.5 parts by weight are added.

In addition, by adding chitosan, the third component of the present invention, to the impression material powder, the number of microorganisms present in the gingival and gingival epithelium after taking the impression due to the antibacterial action of chitosan itself can be reduced, thereby preventing secondary infection and cross infection of dental workers. It can prevent. The chitosan has an advantage in that it is excellent in biocompatibility and hardly toxic to the human body. The chitosan slightly increases mechanical strength such as compression strain and elastic recovery rate of the dental alginate impression material composition, but causes fluorine emission and compression strength to decrease. The content is limited to 1 to 2.5 parts by weight based on 100 parts by weight of the impression material powder.

Since the chitosan is added to the dental alginate impression material powder and must be dissolved in water in order to exhibit antimicrobial properties during use, it is water-soluble or partially water-soluble. Uniform and proper mixing with the impression material powder can effectively exhibit the antibacterial effect of chitosan. The chitosan can be used as long as it has a molecular weight of about 1000 to 100,000 known to exhibit antimicrobial properties, and the present invention does not limit the specific range.

As described above, the present invention can add a impression material powder, a fluorine compound and chitosan to obtain a dental alginate impression material composition.

Method for producing the dental alginate impression material composition may be used a method commonly used in this field, it is not particularly limited in the present invention.

For example, the impression material raw material powder, fluorine compound and chitosan are further added, uniformly mixed by a ball mill, and sieved to obtain a impression material powder of homogeneous particle size,

The water / powder ratio is 10-15 cc of water or fluorine aqueous solution, preferably 12 cc, is mixed with the impression material powder with respect to 1 g of the impression material powder, and is used for taking the impression in the oral cavity.

According to the above-described manufacturing method in the present invention was prepared for the dental alginate impression material composition of various compositions, the physical properties were measured by the International Organization for Standardization.

As a result, fluorine or chitosan was added to the impression material powder (I) or (II) containing medium viscosity or high viscosity sodium alginate as an additive to measure physical properties such as compressive strain and elastic recovery rate (Examples 1 to 16), (Lee Yong-geun, Lim Beom-soon, Kim Cheol-wi: A Study on the Localization and Improvement of Dental Alginate Impression Material, I. Effect of Composition on Characteristics, Journal of Korean Dental Materials, 261-270, 2001) Compared with the alginate impression material powder (I) and (II) which did not add chitosan (Comparative Examples 1-4), the numerical value equivalent or more was obtained. However, in some compositions, the compressive strain and elastic recovery rate tended to change slightly as fluorine and chitosan were added, but all of them were within a significant range and showed a value within or above the range defined in the specification (see Table 1).

Moreover, the surface state after hardening was also confirmed smooth.

In addition, as a result of measuring the amount of fluorine emission with respect to the prepared composition, the amount of the emission was small when it was mixed with an aqueous solution of fluorine, and a high amount was released when it was mixed in the form of soda fluoride powder.

Moreover, as a result of cytotoxicity test to determine the biocompatibility of the composition, it was found to be almost the same as a commercially available product, and the antimicrobial properties of chitosan added were superior to those of the alginate impression material without chitosan. It was confirmed.

As described above, the dental alginate impression material composition presented in the present invention not only has excellent basic properties such as compressive strain, elastic recovery rate, and biocompatibility that the impression material should have, but also has the fluorine release and antibacterial action that conventional products do not have. Given its functionality, it can be used to obtain impressions in dental procedures.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are merely examples for illustrating the present invention, and the present invention is not limited thereto.

% Used below means parts by weight.

Example 1 Preparation of Dental Alginate Impression Material Composition 1

To prepare a basic composition of the dental alginate impression material powder of the present invention was carried out as follows.

1% sodium fluoride powder was added to the medium-weight impression material powder (I) (Wako, 300-400 cp) and mixed homogeneously for 4 hours at a rotational speed of 160 RPM using a ball mill (Young Hana, Korea). The obtained mixed powder was obtained by hitting the standard No. 140 (100 μm) to a certain size, and then mixed with water in an automatic mixer (Combination unit, Whip-mix, USA) for 10 seconds to prepare an alginate impression material composition. At this time, the coma ratio was 12 g of water in 5 g of powder.

Example 2 Preparation of Dental Alginate Impression Material Composition 2

An alginate impression material composition was prepared in the same manner as in Example 1, except that 2% of sodium fluoride was added to the medium-weight impression material powder (I) (Wako, 300-400 cp).

Example 3 Preparation of Dental Alginate Impression Material Composition 3

An alginate impression material composition was prepared in the same manner as in Example 1, except that 1% of sodium fluoride was added to the medium-weight impression material powder (II) (Wako, 300-400 cp).

Example 4 Preparation of Dental Alginate Impression Material Composition 4

An alginate impression material composition was prepared in the same manner as in Example 1, except that 2% of sodium fluoride was added to the medium-weight impression material powder (II) (Wako, 300-400 cp).

Example 5 Preparation of Dental Alginate Impression Material Composition 5

An alginate impression material composition was prepared in the same manner as in Example 1, except that 1% of sodium fluoride was added to the high viscosity impression material powder (I) (Wako, 500 to 600 cps).

Example 6 Preparation of Dental Alginate Impression Material Composition 6

An alginate impression material composition was prepared in the same manner as in Example 1, except that 2% of sodium fluoride was added to the high viscosity impression material powder (I) (Wako, 500 to 600 cps).

Example 7 Preparation of Dental Alginate Impression Material Composition 7

An alginate impression material composition was prepared in the same manner as in Example 1, except that 1% fluorite was added to the high viscosity impression material powder (I) (Wako, 500 to 600 cps).

Example 8 Preparation of Dental Alginate Impression Material Composition 8

An alginate impression material composition was prepared in the same manner as in Example 1, except that 1% of sodium fluoride was added to the high viscosity impression material powder (II) (Wako, 500 to 600 cps).

Example 9 Preparation of Dental Alginate Impression Material Composition 9

An alginate impression material composition was prepared in the same manner as in Example 1, except that 2% of sodium fluoride was added to the high viscosity impression material powder (II) (Wako, 500 to 600 cps).

Example 10 Preparation of Dental Alginate Impression Material Composition 10

An alginate impression material composition was prepared in the same manner as in Example 1, except that 1% fluorite was added to the high viscosity impression material powder (II) (Wako, 500 to 600 cps).

Example 11 Preparation of Dental Alginate Impression Material Composition 11

Except for adding 1% of sodium fluoride to the medium-weight impression material powder (I) (Wako, 300-400 cp) and additionally adding 2% of water-soluble chitosan (young chito, edible product from Koryochito Co., Ltd.). And, in the same manner as in Example 1 to prepare an alginate impression material composition.

Example 12 Preparation of Dental Alginate Impression Material Composition 12

Except for adding 1% of sodium fluoride to the medium-weight impression material powder (II) (Wako, 300-400 cp) and additionally adding 2% of water-soluble chitosan (Youngchito, edible product of Koryochitosan Co., Ltd.). And, in the same manner as in Example 1 to prepare an alginate impression material composition.

Example 13 Preparation of Dental Alginate Impression Material Composition 13

1% sodium fluoride was added to the medium-weight impression material powder (II) (Wako, 300-400 cp), and 2% partially water-soluble chitosan (1% water soluble, manufactured by Koryo Chitosan Co., Ltd.) was additionally added. Except, in the same manner as in Example 1 to prepare an alginate impression material composition.

Example 14 Preparation of Dental Alginate Impression Material Composition 14

Except for adding 1% Sodium Fluoride to high viscosity impression material powder (I) (Wako, 500-600 cp) and additionally adding 2% water-soluble chitosan (1% water-soluble, manufactured by Koryo Chitosan Co., Ltd.). , Alginate impression material composition was prepared in the same manner as in Example 1.

Example 15 Preparation of Dental Alginate Impression Material Composition 15

Except for adding 1% of sodium fluoride to high viscosity impression material powder (II) (Wako, 500-600 cp), and additionally adding 2% of water-soluble chitosan (young chito, edible product from Koryochito Co., Ltd.). , Alginate impression material composition was prepared in the same manner as in Example 1.

Example 16 Preparation of Dental Alginate Impression Material Composition 16

Except for adding 1% of sodium fluoride to high viscosity impression material powder (II) (Wako, 500-600 cp) and additionally adding 2% partially water-soluble chitosan (1% water-soluble, manufactured by Koryo Chitosan Co., Ltd.). And, in the same manner as in Example 1 to prepare an alginate impression material composition.

<Comparative Example 1> Preparation of calcium phosphate-based composite composition 1

The alginate impression material composition was prepared in the same manner as in Example 1 using the medium-weight impression material powder (I) (Wako, 300-400 cp).

Comparative Example 2 Preparation of Calcium Phosphate Composite Composition 2

An alginate impression material composition was prepared in the same manner as in Example 1 using medium viscosity impression material powder (II) (Wako, 300-400 cp).

Comparative Example 3 Preparation of Calcium Phosphate Composite Composition 3

An alginate impression material composition was prepared in the same manner as in Example 1 using high viscosity impression material powder (I) (Wako, 500-600 cp).

Comparative Example 4 Preparation of Calcium Phosphate Composite Composition 4

An alginate impression material composition was prepared in the same manner as in Example 1 using high viscosity impression material powder (II) (Wako, 500-600 cp).

The compositions of Examples 1 to 16 and Comparative Examples 1 to 4 are shown in Table 2 below.

Furtherance Impression material powder (parts by weight) Fluorine compound (part by weight) Chitosan (part by weight) Mixed Composition (Ⅰ) ¹⁾ Mixed composition (Ⅱ) ²⁾ Soda Fluoride Fluoride Water soluble chitosan Partially water-soluble chitosan Midpoint ³⁾ High viscosity ⁴⁾ Midpoint High viscosity Example 1 100 - - - One - - - Example 2 100 - - - 2 - - - Example 3 - 100 - - One - - - Example 4 - 100 - - 2 - - - Example 5 - - 100 - One - - - Example 6 - - 100 - 2 - - - Example 7 - - 100 - - One - - Example 8 - - - 100 One - - - Example 9 - - - 100 2 - - - Example 10 - - - 100 One - - Example 11 100 - - - One - 2 - Example 12 - 100 - - One - 2 - Example 13 - 100 - - One - 2 Example 14 - - 100 - One - 2 - Example 15 - - - 100 One - 2 - Example 16 - - - 100 One - - 2 Comparative Example 1 100 - - - - - - - Comparative Example 2 - 100 - - - - - - Comparative Example 3 - - 100 - - - - - Comparative Example 4 - - - 100 - - - - 1) Mixed composition (I): sodium alginate 11.35%, calcium sulfate 11.55%, diatomaceous earth 65.6%, borax 1.9%, magnesium oxide 1.9%, potassium chloride 1.9%, sodium acetate 1.9%, sodium phosphate 2.0%, zinc fluoride 1.9%, Zinc oxide 1.9% .2) Mixed composition (II): sodium alginate 11.35%, calcium sulfate 11.55%, diatomaceous earth 65.6%, borax 1.9%, magnesium oxide 1.9%, sodium acetate 1.9%, sodium phosphate 2.0%, zinc fluoride 1.9% Zinc oxide 1.9%. 3) Medium viscosity sodium alginate: 300-400 cp4) High viscosity sodium alginate: 500-600 cp

In order to examine the properties of the calcium phosphate-based composites obtained in Examples 1 to 16 and Comparative Examples 1 to 4, International Organization for Standardization (ISO, 1990) 1563, Korean Dental Association Standard No. 8, Korean Industrial Standards (KS) P74191, Korea Food and Drug Administration Notice (KFDA) No. 1 and American Dental Association Standard No. 18 (1992) were evaluated.

Experimental Example 1

1) Compression strain and elastic recovery

It was measured according to ISO 6.6 363 strain at compression.

The specimen was placed on a compression mechanism, stressed at 0.01 N / mm 2 on it, the height was read, and then the force was increased to 1,250 ± 10 g to read the height as the strain at compression (compression strain).

Recovery after deformation (elastic recovery rate) was tested in accordance with the standard 6.5, these results are shown in Table 3 below.

Example Compression Strain (%) Elastic recovery rate (%) Example 1 15.45 (1.81) 93.18 (0.36) Example 2 15.64 (1.42) 93.33 (0.24) Example 3 17.04 (1.53) 93.00 (0.16) Example 4 16.52 (1.07) 92.19 (0.45) Example 5 17.34 (2.07) 93.24 (0.29) Example 6 17.91 (1.52) 92.43 (0.32) Example 7 18.48 (2.69) 92.76 (0.24) Example 8 18.87 (1.05) 92.82 (0.39) Example 9 19.62 (0.90) 92.57 (0.18) Example 10 17.73 (0.84) 93.37 (0.69) Example 11 20.75 (2.13) 92.33 (0.33) Example 12 20.48 (2.70) 92.04 (0.24) Example 13 19.19 (1.59) 92.07 (0.43) Example 14 19.19 (1.77) 92.23 (0.20) Example 15 16.38 (1.21) 92.96 (0.48) Example 16 17.99 (1.79) 93.00 (0.57) Comparative Example 1 12.75 (1.11) 94.03 (0.10) Comparative Example 2 19.20 (1.32) 93.69 (1.80) Comparative Example 3 17.73 (2.28) 93.09 (0.55) Comparative Example 4 18.45 (0.93) 93.45 (0.71) * Compressive strain refers to flexibility, which is defined as 5-20%, and elastic recovery rate (= 100-permanent strain) is defined as 95% or more.

According to Table 3, the composition using the fluorine compound in the impression material powder (I) containing a medium viscosity sodium alginate was all 15 to 18% in the compressive strain, all of which meet the standard, in addition to the composition of the water-soluble chitosan or partially water-soluble chitosan In addition, it showed a compressive strain of up to 20%, which was in compliance with the International Organization for Standardization. In addition, the composition to which fluorine was added showed a tendency for the elastic recovery rate to fall slightly compared with the composition without addition.

Also in the composition containing impression material powder (II) containing a medium viscosity sodium alginate, the compressive strain obtained the preferable result of less than 20%, and the elastic recovery rate did not change significantly even if fluorine was added.

The composition containing the impression material powder (Ⅰ) containing high viscosity sodium alginate also met the standard with a compressive strain of less than 20%. The addition of fluorine solution and chitosan resulted in slightly increased results, but it was used as an impression material. It was not as significant as it could not be. In addition, there was no significant change in the elastic recovery rate even when fluorine was added.

Finally, the composition containing the impression material powder (II) containing high viscosity sodium alginate, like the impression material powder (I) containing high viscosity sodium alginate resulted in a slight increase in compression strain when additional fluorine solution and chitosan were added. It was shown that the numerical value falls within the error range and less than 20% for all the remaining compositions were found to comply with the standard. In addition, the elastic recovery rate did not change significantly even if fluorine or chitosan was added.

As a result, it was found that the compressive strain and the elastic recovery rate were almost equivalent to those of the compositions of Comparative Examples 1 to 4, which are conventionally commercially available.

2) curing time

It was measured according to <6.4 Initial Curing Time> of Part 18 of the American Dental Association.

The alginate sample preparation mold was injected with the alginate impression material composition of Example or Comparative Example prepared above, and immediately contacted the flat end of the polished poly (methylmethacrylate) rod 6 mm in diameter and 10 cm in length at 10 second intervals, and separated cleanly. Continued until At this time, the hardening time was the time from the start of mixing until the impression material was not buried at the end of the rod. In the case of commercially available products, curing within 15 seconds of the manufacturer's suggested time is considered to comply with the standard.

division Curing time (minutes) division Curing time (minutes) Example 1 2.03 (± 0.31) Example 11 1.89 (± 0.10) Example 2 2.33 (± 0.14) Example 12 2.33 (± 2.24) Example 3 1.92 (± 0.20) Example 13 2.75 (± 0.12) Example 4 1.89 (± 0.38) Example 14 1.89 (± 0.10) Example 5 2.25 (± 0.10) Example 15 2.42 (± 0.12) Example 6 1.88 (± 0.25) Example 16 2.00 (± 0.24) Example 7 2.06 (± 0.25) Comparative Example 1 2.92 (± 0.22) Example 8 2.08 (± 0.32) Comparative Example 2 1.79 (± 0.08) Example 9 1.92 (± 0.23) Comparative Example 3 3.25 (± 0.69) Example 10 2.00 (± 0.26) Comparative Example 4 1.88 (± 70.21)

According to Table 4, the curing time was similar to the commercial product about 2 to 3 minutes. The curing time of the product of the present invention may vary depending on the composition, but may be presented in about 2 to 3 minutes. In the above table, curing time 1.51 minutes means 1 minute 30 seconds.

3) Fluorine emission amount measurement

The alginate impression material composition (0.5 g) obtained in the said Example or the comparative example was mixed with distilled water or a fluorine solution (1.2 mL), and it injected | poured into the Teflon mold of diameter 6mm and height 2mm, and prepared the test piece. Three specimens and 3 ml of distilled water were added to a 15 ml test tube and mixed with a Vortex mixer for 5 minutes. Then, the specimens were removed and the solution was transferred to a 50 ml test tube and mixed with Tisab in a 1: 1 ratio with a Vortex mixer for 20 seconds. The solution was placed in a constant temperature water bath and the temperature was adjusted to 20-23 ° C. to measure fluorine emission using an ion analyzer (pH / ion meter, DP-88oM, Dongwoo Medical). The results are shown in Table 5 below.

Fluorine Emissions (PPM) Fluorine Emissions (PPM) Example 1 10.120 (± 1.852) Example 11 11.616 (± 0.914) Example 2 14.371 (± 1.033) Example 12 7.383 (± 0.276) Example 3 10.457 (± 0.980) Example 13 6.256 (± 0.237) Example 4 13.168 (± 1.652) Example 14 5.387 (± 0.300) Example 5 11.867 (± 2.600) Example 15 10.318 (± 0.436) Example 6 14.761 (± 1.507) Example 16 10.214 (± 0.397) Example 7 6.808 (± 0.230) Comparative Example 1 0.702 (± 0.023) Example 8 13.932 (± 1.793) Comparative Example 2 0.652 (± 0.063) Example 9 12.592 (± 1.980) Comparative Example 3 0.438 (± 0.010) Example 10 6.771 (± 0.250) Comparative Example 4 0.441 (± 0.039)

According to Table 5, the fluorine emission amount of the composition of the Example was about 6 to 14 ppm, while the composition of the comparative example showed a low value of 0.4 to 0.7 ppm. The amount of fluorine emission was different depending on the materials and methods to be added, but when mixed with 100 ppm aqueous fluorine solution, there was no significant difference from the case of mixing with distilled water. High fluoride emission (p = 0.05) In addition, the amount of fluorine emission when fluorine was added to the impression material to which chitosan was added was similar to that when chitosan was not added. In this case, the mixture of 100 ppm aqueous fluorine solution was significantly higher than that of distilled water. Seemed.

4) Compression Characteristics

The experiment was conducted based on ISO 6.7 6 compressive strength.

After 60 seconds of curing, the specimens prepared with the compositions of the above examples and the comparison were placed on paper at both ends of the specimens, placed on the measuring section of a compression-tension tester (Instron 4465, England), and loaded at a rate of 10 mm per minute. The compressive strength, the maximum strain during compression (strain from the start of the load to the point where the elastic modulus starts to rise sharply on the stress-strain curve) and the elastic modulus were measured, and the results are shown in Table 6 below.

Compressive strength (MPa) Maximum strain at compression (%) Modulus of elasticity (MPa) Example 1 0.839 (± 0.124) 80.321 (± 18.112) 1.553 (± 0.198) Example 2 0.690 (± 0.083) 79.582 (± 9.865) 2.079 (± 0.383) Example 3 0.788 (± 0.053) 74.017 (± 12.813) 1.298 (± 0.198) Example 4 0.493 (± 0.170) 80.761 (± 11.880) 0.928 (± 0.251) Example 5 0.703 (± 0.116) 75.202 (± 2.842) 1.376 (± 0.263) Example 6 0.457 (± 0.049) 74.918 (± 5.481) 1.082 (± 0.340) Example 7 1.059 (± 0.117) 85.396 (± 2.318) 1.397 (± 0.461) Example 8 0.618 (± 0.074) 72.405 (± 0.884) 1.556 (± 0.023) Example 9 0.488 (± 0.037) 72.855 (± 3.311) 0.732 (± 0.116) Example 10 0.921 (± 0.175) 85.436 (± 4.569) 1.491 (± 0.451) Example 11 0.522 (± 0.076) 70.738 (± 1.253) 1.412 (± 0.122) Example 12 0.453 (± 0.078) 74.628 (± 3.945) 1.049 (± 0.364) Example 13 0.512 (± 0.071) 74.340 (± 0.525) 1.267 (± 0.157) Example 14 0.483 (± 0.042) 73.259 (± 2.501) 1.148 (± 0.123) Example 15 0.547 (± 0.052) 72.007 (± 0.722) 1.299 (± 0.133) Example 16 0.491 (± 0.030) 80.896 (± 4.075) 1.004 (± 0.122) Comparative Example 1 1.261 (± 0.197) 84.190 (± 4.312) 4.304 (± 1.167) Comparative Example 2 1.246 (± 0.098) 89.128 (± 2.814) 1.211 (± 0.130) Comparative Example 3 1.053 (± 0.145) 87.061 (± 4.280) 1.861 (± 0.263) Comparative Example 4 1.013 (± 0.262) 86.110 (± 2.908) 1.272 (± 0.096)

According to Table 6, when fluorine was added to the impression material powder (I) containing a medium viscosity sodium alginate, the compressive strength was 0.690 to 1.261 MPa, which was higher than 0.35 MPa suggested in the specification. In the case of the addition of chitosan, 2% sodium fluoride or fluorite, the modulus of elasticity was significantly lowered and the modulus of elasticity was lowered after addition of fluorine and chitosan. This tendency was similar when fluorine and chitosan were added to impression material powder (II) containing medium viscosity sodium alginate, impression material powder (I) and (II) containing high viscosity sodium alginate.

As a result, the maximum strain at the time of compression was slightly different depending on the blending ratio of 70 to 80%, the elastic modulus of the embodiment according to the present invention did not have a large difference around 1 MPa.

5) Micropart Reproducibility

In order to examine the reproducibility of the micro parts in the case of using the alginate impression material composition obtained in the above Examples and Comparative Examples as the impression material was performed as follows.

The affinity with the gypsum and the reproducibility of the micro parts were evaluated to the extent of reproducing 50 mm of lines at 25 mm, and Crystal Rock (Maruish Gypsum Co. Japan) was used as hard stone. The impression was obtained using the alginate impression material compositions of Examples and Comparative Examples and compared with the case where the model material was injected after immersion in 2% potassium sulfate solution for 1 minute.

As a result, micro-part reproducibility was reproduced with 50 µm lines in all materials, and after the impression was taken, after immersion in 2% potassium sulphate solution for 1 minute and then the model was injected, it was visually judged that the surface was not immersed. It showed a smoother surface.

6) Change in acidity during curing

Neutrality was maintained even when the fluorine compound or chitosan used in the present invention was added, and the change in pH over time of the alginate impression material powder was measured and the results are shown in FIG. 1. According to Figure 1, the commercial product after 5 minutes of mixing was acidic to about 4, but the alginate of the present invention was confirmed to maintain the neutrality, as a result of the impression material composition of the present invention can improve the affinity with the gypsum model It can be predicted sufficiently.

7) Viscosity change during curing

When the fluorine compound and chitosan used in the present invention were added, the viscosity tended to increase slightly over time, and the change in viscosity with time was measured for the alginate impression material powder added with chitosan. Indicated.

Chitosan was added to the impression material powder composition (I) containing mid-range sodium alginate to measure the viscosity over time (see FIG. 2), and the initial viscosity was higher than that of the composition without chitosan and increased with time. Showed a tendency to. The initial viscosity is a viscosity immediately after mixing, and indicates the fluidity of the impression material, and the rate at which the viscosity increases means a curing time.

However, the viscosity was slightly higher than that without addition at the same time after chitosan mixing, but the curing time was similar to that before addition.

Experimental Example 2 Measurement of Biocompatibility and Antimicrobial Effect

In order to determine the biocompatibility of the dental alginate impression material composition of the present invention was measured by the MTT method and the antimicrobial effect was measured.

1) Cytotoxicity Test

(1) Cell culture

L929 cells (NCTC clone 929; L-929, No. of KCLB 10001) were used. In a 10% fetal bovine serum with 10,000 U / ml penicillin G sodium and 10,000 μg / ml streptomycin sulfate in RPMI 1640 at 37 ° C. and 5% CO ₂ incubator. ) (Gibco Co, USA) was added to the culture medium.

(2) MTT assay

Cells of 5 × 10 ⁴ were diluted in 15 ml culture solution and 100 µl each of the 96 well culture dishes was incubated for 24 hours. The cytotoxicity evaluation material was mixed and placed in a Teflon mold having a diameter of 6.0 mm and a height of 1.8 mm, cured for 1 hour, removed from the mold, and added to a culture medium without adding 2 ml of FBS per specimen and stirred at 37 ° C. for 24 hours. After the solid was removed and sterilized using a 0.20-㎛ filter. 50 μl per well of the culture dish was added to the extract, and the resultant was incubated for 24 hours, followed by MTT solution. The MTT solution was dissolved in PBS at 5 mg / ml and filtered using a 0.20-μm filter. 16.5 μl MTT solution (final MTT concentration was 0.5 mg / ml) was added to each well and incubated at 37 ° C. and 5% CO ₂ for 4 hours. After the culture solution was left with about 30 μl, 100 μl of DMSO was added to each well, and the resultant was allowed to stand for 18 minutes. The absorbance at 540 nm was measured using an ELISA reader.

The results of the dehydrogenase activity of the mitochondria compared with the negative control group as a ratio are shown in Table 7 below. At this time, the negative control group was used for extracting the same size of Teflon stirred for 24 hours, and the positive control group was mixed with zinc oxide and eugenol 5: 1 to produce the same size specimen and extracted under the same conditions Used.

division Cytotoxicity (ratio to negative control) Example 11 0.512 (± 0.140) Example 12 0.501 (± 0.192) Example 13 0.494 (± 0.160) Example 14 0.747 (± 0.044) Example 15 0.734 (± 0.073) Example 16 0.761 (± 0.057) Comparative Example 1 0.667 (± 0.060) Comparative Example 2 0.487 (± 0.023) Comparative Example 3 0.635 (± 0.103) Comparative Example 4 0.629 (± 0.116)

According to Table 7, when the water-soluble chitosan was added to the impression material powder composition (I) and (II), the cell activity (succinyl dehydrogenase, an intracellular enzyme) for the negative control group was found to be 0.501 to 0.814. When the water-soluble chitosan was added, the cytotoxicity was generally high at 0.494 to 0.767.

2) antimicrobial test

In order to determine the antimicrobial activity of the alginate impression material composition according to the present invention was measured as follows. The antimicrobial activity was measured by adding 2% of water-soluble chitosan and partially water-soluble chitosan to the impression material powder composition (I) containing mid-range sodium alginate, and the powder composition (I) to which nothing was added was used as a control.

Each composition was prepared with a specimen of dental alginate impression material having a diameter of 6 mm and a height of 1.5 mm by using a Teflon mold. Within 30 minutes, 5 pieces of specimens were placed in 1 ml of broth media and inoculated with the bacteria at regular intervals. Was collected. Subsequently, the plate was inoculated in a nutrient medium using a spiral plater (Autoplate 4000, Spiral Biotech, USA), and cultured for 12 hours at 3 hour intervals. At this time, E. coli and Staphylococcus aureus were used as strains, and the liquid medium containing the sample was inoculated by diluting 10,000 times.

64.3 × 10 ³ CFU / mL after 3 hours with E. coli , 66.2 × 10 ³ CFU / mL after 6 hours, 21.1 × 10 ³ CFU / mL after 9 hours, and 14.3 after 12 hours × 10 ³ CFU / mL was shown, indicating that the antibacterial property was very excellent. Similar results were also obtained in the experiments with partially water-soluble chitosan, which was superior to the case with the addition of water-soluble chitosan when the results were compared at the same time at 23.1 × 10 ³ CFU / mL after 6 hours.

However, in the antimicrobial test of S. aureus , the addition of chitosan did not have a clear effect on the antimicrobial activity.

As described above, in the present invention, a new composition was prepared by adding a fluorine compound and chitosan to the dental alginate impression material powder, and as a result of measuring various physical properties of the composition, it was possible to obtain a result equivalent to or higher than that of a conventionally used product. In particular, the fluorine emission is excellent and the fluorine is applied to the tooth during the impression taking process, and after the impression is taken, the number of microorganisms remaining in the impression material is reduced. It is very suitable as alginate impression material.

Claims (6)

Sodium alginate, calcium sulfate, diatomaceous earth, borax, magnesium oxide, potassium chloride, sodium acetate, sodium acetate per 100 parts by weight of the impression material powder containing phosphate) and zinc fluoride, 0.5 to 2.5 parts by weight of sodium fluoride, a fluorine compound, and 0.5 to 1.5 parts by weight or a mixture thereof; And A multifunctional dental impression material composition comprising 1 to 2.5 parts by weight of a water-soluble or partially water-soluble chitosan powder. According to claim 1, wherein the impression material powder Sodium alginate 11.35 wt%, calcium sulfate 11.55 wt%, diatomaceous earth 65.6 wt%, borax 1.9 wt%, magnesium oxide 1.9 wt%, potassium chloride 1.9 wt%, sodium acetate 1.9 wt%, sodium phosphate 2.0 wt% and zinc fluoride 1.9 wt% Impression material composition, characterized in that it contains%. Sodium alginate, calcium sulfate, diatomaceous earth, borax, magnesium oxide, sodium acetate, sodium phosphate, zinc fluoride Based on 100 parts by weight of the impression material powder containing fluoride and zinc oxide, 0.5 to 2.5 parts by weight of sodium fluoride, a fluorine compound, and 0.5 to 1.5 parts by weight or a mixture thereof; And A multifunctional dental impression material composition comprising 1 to 2.5 parts by weight of a water-soluble or partially water-soluble chitosan powder. The method of claim 3, wherein the impression material powder Sodium alginate 11.35 wt%, calcium sulfate 11.55 wt%, diatomaceous earth 65.6 wt%, borax 1.9 wt%, magnesium oxide 1.9 wt%, sodium acetate 1.9 wt%, sodium phosphate 2.0 wt%, zinc fluoride 1.9 wt% and zinc oxide 1.9 wt% Impression material composition, characterized in that contained in%. The impression material composition according to any one of claims 1 to 4, wherein the sodium alginate has a medium viscosity of 300 to 400 cp or high viscosity of 500 to 600 cp. The impression material composition according to any one of claims 1 to 4, wherein the impression material powder has a size of 100 µm or less.