JPH04364174A - Indicator composition for detecting sterilization - Google Patents

Abstract

PURPOSE:To obtain the subject composition containing a transition metal compound, sulfur, monoazo dye, organic acid, etc., as active ingredients and capable of corresponding to both of autoclave sterilization and ethylene oxide gas sterilization in medical field. CONSTITUTION:2-15 pts.wt. transition metal compound (e.g. bismuth oxide) is mixed with 5-30 pts.wt. sulfur or a sulfur compound (e.g. 1,3- diphenyl-2-thiourea), 0.1-3.5 pts.wt. monoazo dye expressed by the formula (R<1> is H, methyl, ethyl or acylamino; R<2> is H, methoxy or ethoxy; R<3> to R<5> are H, OH, nitric acid or 1-4C alkyl) and 1-15 pts.wt. organic acid or metal salt of organic acid (e.g. calcium salicylate). Then, a vehicle for ink is added to the mixture and these components are blended and made into ink by a dispersing machine to prepare the indicator composition. The composition is reacted with both of high pressure steam and ethylene oxide gas to provide the objective indicator having color changing property capable of displaying sterilization state.

Description

[Detailed description of the invention]

0001

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sterilization detection indicator composition suitable for detecting and confirming sterilization conditions in autoclave sterilization and ethylene oxide gas sterilization for, for example, sterilizing medical equipment.

0002

2. Description of the Related Art Autoclave sterilization, which involves heating with high-pressure steam for a certain period of time, and gas sterilization, which uses ethylene oxide gas, are popular methods for sterilizing medical instruments in the medical field. To confirm the completion of sterilization process,
For example, B. subtilis and heat-resistant bacteria (B. subtilis).
There are two methods: one method is to use a biochemical indicator such as Stearothermophilus, and the other is to use a chemical indicator that changes color in response to an atmosphere such as high-pressure steam or ethylene oxide gas.

[0003] The former biochemical indicator allows accurate confirmation, but it requires culturing of the treated bacteria and it takes time to determine the sterilization process, so the latter chemical indicator, which is easier to handle, is used. There are many. A chemical indicator is one in which an indicator composition that changes color in response to high-pressure steam or an indicator composition that changes color in response to ethylene oxide gas is applied to a substrate such as paper or a plastic film. The quality of the sterilization process is determined by the change in color. Japanese Patent Publication No. 61-287972
No. 2-180973 discloses an indicator that changes color in response to high-pressure steam. Special Publication No. 52-10043 and Special Publication No. 57-4
No. 0869 discloses an indicator composition that changes color in response to ethylene oxide gas.

However, the composition used in such an indicator reacts only with either high-pressure steam or ethylene oxide gas. In actual sterilization work, it is necessary to prepare both an indicator dedicated to autoclave sterilization processing and an indicator dedicated to ethylene oxide gas sterilization processing, and to use them depending on the sterilization method, which is inconvenient. If the indicator is used incorrectly, sterilization cannot be confirmed and the product must be re-sterilized.
We are forced into waste and complexity. Furthermore, it is necessary to prepare separate indicators depending on the sterilization method, which tends to complicate inventory management.

[0005]

[Problems to be Solved by the Invention] The present invention has been made to solve the above-mentioned problems, and is compatible with both autoclave sterilization and ethylene oxide gas sterilization in the medical field, and is compatible with each sterilization processing condition. An object of the present invention is to provide an indicator composition for sterilization detection that has color-changing properties.

[0006]

[Means for Solving the Problems] In order to achieve the above object, the present inventors aimed to obtain an indicator composition that can be used as both an indicator for detecting autoclave sterilization and an indicator for detecting ethylene oxide gas sterilization. As a result of extensive research, it was discovered that the composition shown below meets the above objectives, and the present invention was completed.

That is, the sterilization detection indicator composition of the present invention contains 2 to 15 parts by weight of one or more transition metal compounds and at least one of sulfur and sulfur compounds in 100 parts by weight of the composition. 5 to 30 parts by weight, general formula

[0008]

[Case 2]

Contains 0.1 to 3.5 parts by weight of one or more monoazo dyes represented by: and 1 to 15 parts by weight of at least one of an organic acid and a metal salt of an organic acid. .

R1 in the formula is a hydrogen group, a methyl group, an ethyl group or an acylamino group. R2 is a hydrogen group, a methoxy group or an ethoxy group. R3, R4, and R5 are a hydrogen group, a hydroxyl group, a nitric acid group, an alkyl group having 1 to 4 carbon atoms, an alkyl group having 1 to 4 main chain carbon atoms substituted with an acyloxy group, and a main chain carbon number substituted with a cyano group. It is an alkyl group having 1 to 4 carbon atoms, or an alkyl group having 1 to 4 carbon atoms in the main chain substituted with an alkoxy group.

[0011] The transition metal compound constituting the composition, sulfur,
Sulfur compounds are components that change color when exposed to high pressure steam.

Examples of transition metal compounds include basic carbonates, hydroxides, oxides, and stearic acid compounds of nickel, cobalt, copper, lead, and bismuth. A suitable content of the transition metal compound is 2 to 1 of the total amount of the composition.
5 parts by weight, preferably 5 to 10 parts by weight. When the content of the transition metal compound is 2 parts by weight or less, the color difference before and after the color change is small, and the color change is difficult to notice. If the amount is 15 parts by weight or more, the adhesion to the printing material when made into ink is reduced, causing the problem of contaminating the material to be sterilized during sterilization.

[0013] As the sulfur compound, inorganic or organic sulfur compounds can be used. Examples of inorganic sulfur compounds include zinc sulfide. Examples of organic sulfur compounds include thiourea, methylthiourea, 1-phenyl-2-thiourea, 1,3-diphenyl-2-thiourea, 2,2'-
Ditolylthiourea and o-tolylthiourea are mentioned. A suitable content of sulfur or sulfur compounds is 5 to 30 parts by weight, preferably 8 to 15 parts by weight, based on the total amount of the composition. When the content of sulfur or sulfur compounds is 5 parts by weight or less, the difference in color before and after the color change is small, and the color change is difficult to notice. If the amount is 30 parts by weight or more, the adhesion to the printing material when made into ink is reduced, causing the problem of contaminating the material to be sterilized during sterilization.

[0014] The monoazo dye, organic acid,
The metal salt of an organic acid is a component that changes color when exposed to ethylene oxide gas.

Examples of monoazo dyes having the structure of the above formula include C.I. I. (Color Index) Discharge Red 58, C. I. discharge red 88,
C. I. Discharge Red 110, C. I. Discharge Red 117, C. I. Discharge Red 137, C. I. discharge violet 43
,C. I. Discharge Blue 102 is an example. A suitable content of monoazo dye is 0.1 of the total amount of the composition.
-3.5 parts by weight, preferably 0.5-1.5 parts by weight. When the content of the monoazo dye is 0.1 part by weight or less, the coloring power during printing is reduced and the color of the indicator itself becomes pale. When the amount is 3.5 parts by weight or more, the discoloration property decreases, and the change in color due to sterilization becomes small.

Examples of organic acids include acrylic acid, adipic acid, L-aspartic acid, azelaic acid, benzoic acid, anthranilic acid, isophthalic acid, itaconic acid, undecylenic acid, citric acid, glutaconic acid, cresotic acid,
Salicylic acid, cyanuric acid, diglycolic acid, DL-tartaric acid, sulfanilic acid, sebacic acid, sorbic acid, terephthalic acid, naphthenic acid, nicotinic acid, hippuric acid, barbituric acid, pivalic acid, pyruvic acid, phthalic acid, fumaric acid,
Mention may be made of benzylic acid, maleic acid, malonic acid, methacrylic acid and metanilic acid.

Examples of the metal salts of organic acids include calcium salts, zinc salts, magnesium salts, sodium salts, and potassium salts of the above-mentioned organic acids.

Among them, citric acid, malonic acid, phthalic acid,
Adipic acid, maleic acid, calcium salicylate, zinc salicylate, zinc benzoate and o-cresotinic acid are preferred. The appropriate content of these organic acids and metal salts of organic acids is 1 to 15 parts by weight, preferably 3 to 15 parts by weight based on the total amount of the composition.
It is 10 parts by weight. When the content of the organic acid and the metal salt of the organic acid is 1 part by weight or less, the problem arises that discoloration due to ethylene oxide gas worsens and the detection ability deteriorates. When the amount is 15 parts by weight or more, the storage stability in the ink state decreases.

The indicator composition of the present invention can be prepared by mixing the above-mentioned materials and an ink vehicle by ball milling, roll milling,
It is obtained by mixing and forming into ink using a dispersing machine such as a sand mill.

In addition to the above-mentioned materials, the composition of the present invention contains various additives used in conventional dedicated indicator compositions, including other colored pigments, color enhancers, rust preventives, and surfactants. You may also add For example, by adding silica, barium sulfate, clay, magnesium carbonate, calcium carbonate, etc., the permeability of ethylene oxide gas to the printed composition film can be improved. Furthermore, by adding a dye with excellent heat resistance and gas resistance, the color before and after color change can be adjusted.

The indicator composition thus obtained is formed into a printing ink and printed on a suitable substrate such as high-quality paper, crepe paper, or plastic film to produce a detection card or a detection tape. Or, it can be printed directly on packaging materials for items to be sterilized.

[0022] For the ink vehicle, a resin is used that does not impair the discoloration of the indicator and has excellent adhesion to the printing material. For example, ethyl cellulose, nitrocellulose, butyral resin, acrylic ester resin,
Examples include polyamide resins, phenol resins, and rosin-modified maleic acid resins. Commercially available ink vehicles meeting the above conditions may be used.

[0023]

[Action] The indicator composition for sterilization detection of the present invention changes color by reacting with both high-pressure steam and ethylene oxide gas, and can be sterilized by autoclave sterilization and ethylene oxide sterilization by simply applying it to any base material. An indicator that meets the conditions is manufactured. When the indicator is sterilized in an autoclave, the transition metal compound reacts with sulfur and sulfur compounds under the moist heat conditions to produce metal sulfide, which changes the color of the composition. When sterilized with ethylene oxide gas, the monoazo dye and ethylene oxide gas react and the color of the composition changes. Organic acids and metal salts of organic acids not only promote the reaction between ethylene oxide gas and monoazo dye, but also work to adjust the color change conditions (color change temperature and time until color change).

[0024]

[Examples] Examples of the present invention will be described below. Example 1 Bismuth oxide (Bi2O3)

5.0 parts by weight 1,3-diphenyl-2-thiourea
10.0 parts by weight C. I. discharge red 110
1.0 parts by weight Calcium salicylate
9.0 parts by weight
ethyl cellulose
10.0 parts by weight
butyl cellosolve
65.0 parts by weight The above blend was kneaded in a ball mill for 24 hours to obtain a red ink. A printed matter screen-printed with this ink on high-quality paper turned black when sterilized in an autoclave at 121° C. for 10 minutes. In addition, the same printed matter was treated with a mixed gas of 20% ethylene oxide and 80% carbon dioxide (
When sterilized for 1 hour at a gas pressure of 1.0 kg/cm 2 , a temperature of 50° C., and a relative humidity of 50% RH, the color changed to blue.

Example 2 Basic lead carbonate

6.0 parts by weight sulfur

12.0 parts by weight
C. I. discharge red 117
1.2 parts by weight
malonic acid
4
．． 8 parts by weight S-LEC B BL
-1 (Sekisui Chemical) 6
．． 0 parts by weight isopropyl alcohol
40.0 parts by weight toluene

20.0 parts by weight
methyl cellosolve
10.0 parts by weight of the above blend was kneaded in a sand mill for 30 minutes to obtain a red ink. Prints made by gravure printing this ink on sterile paper are
The color changed to black by autoclave sterilization at 121°C for 5 minutes. In addition, the same printed matter was treated with a mixed gas of 20% ethylene oxide and 80% carbon dioxide (gas pressure 1.0
When sterilized for 3 hours at a temperature of 50° C. and a relative humidity of 50% RH, the color changed to blue.

Example 3 Copper hydroxide

8.0 parts by weight Thiourea

12.0 parts by weight
C. I. discharge red 58
0.8 parts by weight
Zinc benzoate
5.2
Weight part Pass No. 800 medium (manufactured by Jujo Kako) 60.0
Part by weight Butyl cellosolve

14.0 parts by weight The above blend was kneaded in a ball mill for 24 hours to obtain a red ink. A printed matter screen-printed with this ink on high-quality paper turned black when sterilized in an autoclave at 121° C. for 10 minutes. In addition, the same printed matter was mixed with 20% ethylene oxide and 80% carbon dioxide.
% mixed gas (gas pressure 1.0 kg/cm2, temperature 5
When sterilized for 1 hour at 0° C. and 50% RH, the color changed to blue.

Example 4 Basic cobalt carbonate
6.
0 parts by weight Methylthiourea

8.0 parts by weight C. I. discharge red 88
0.6 parts by weight C.
I. pigment yellow 1
3.0 parts by weight
o-cresotic acid
10.4 parts by weight
FBHD medium (manufactured by Toyo Ink)
60.0 parts by weight
FB-702 solvent (manufactured by Toyo Ink)
12.0 parts by weight of the above blend was kneaded in a sand mill for 30 minutes to obtain an orange ink. A printed matter obtained by gravure printing this ink on sterilized paper turned black after being sterilized in an autoclave at 121° C. for 10 minutes. When the same printed matter was sterilized for 3 hours with a mixed gas of 20% ethylene oxide and 80% carbon dioxide (gas pressure 1.0 kg/cm2, temperature 50° C., relative humidity 50% RH), the color changed to green.

Example 5 Basic bismuth carbonate
7.
0 parts by weight 2,2'-ditolylthiourea
11.0 parts by weight C. I. discharge red 137
1.0 parts by weight adipic acid
4.0 parts by weight
o-cresotic acid
1.0 parts by weight magnesium carbonate

2.0 parts by weight Styrene B medium (manufactured by Toyo Ink) 60.0 parts by weight AS-102 solvent (manufactured by Toyo Ink) 14
．． 0 parts by weight The above blend was kneaded in a sand mill for 30 minutes to obtain a red ink. The printed material obtained by flexographic printing with this ink on sterilized paper turned black after being sterilized in an autoclave at 121° C. for 20 minutes. Further, when the same printed matter was sterilized for 1 hour with a mixed gas of 20% ethylene oxide and 80% carbon dioxide (gas pressure 1.0 kg/cm2, temperature 50° C., relative humidity 50% RH), the color changed to blue.

Comparative Example 1 The formulation of Example 1 except for 1,3-diphenyl-2-thiourea was kneaded in a ball mill for 24 hours to obtain a red ink. Printed matter screen-printed with this ink on high-quality paper showed no discoloration when sterilized in an autoclave at 121°C for 30 minutes. In addition, the same printed matter was mixed with 20% ethylene oxide and 80% carbon dioxide.
% mixed gas (gas pressure 1.0 kg/cm2, temperature 5
When sterilized for 3 hours at 0° C. and 50% RH, the color changed to blue.

Comparative Example 2 The formulation of Example 2, excluding malonic acid, was kneaded in a sand mill for 30 minutes to obtain a red ink. Prints made by gravure printing this ink on high-quality paper are heated at 121℃ and 50℃.
The color changed to black after autoclaving for 1 minute. In addition, the same printed matter was treated with a mixed gas of 20% ethylene oxide and 80% carbon dioxide (gas pressure 1.0 kg/cm2).
When sterilized for 3 hours at a temperature of 50° C. and a relative humidity of 50% RH, no discoloration was observed.

In each of the Examples and Comparative Examples, the mixed gas used for ethylene oxide gas sterilization was Daicide H20 manufactured by Daido Sanso Co., Ltd.

[0032]

Effects of the Invention As described above in detail, the indicator composition for sterilization detection of the present invention has a color change property that is consistent with the processing conditions of both autoclave sterilization and ethylene oxide gas sterilization in the medical field. We are prepared. After the object to be sterilized and the indicator using the composition of the present invention are sterilized together, it can be easily detected whether the object to be sterilized has been sterilized under appropriate conditions by observing the discoloration of the indicator. be able to. In this case, there is no need to select an indicator depending on the sterilization method as in the past, and misuse of the indicator is avoided. Further, there is no need to prepare separate indicators depending on the sterilization method, and inventory management can be simplified.

Claims (1)

[Claims] 1. In 100 parts by weight of the composition, 2 to 15 parts by weight of one or more transition metal compounds, 5 to 30 parts by weight of at least one of sulfur and sulfur compounds, and a compound having the general formula 1] [wherein R1 is a hydrogen group, methyl group, ethyl group or acylamino group, R2 is a hydrogen group, methoxy group or ethoxy group, R3, R4 and R5 are a hydrogen group, a hydroxyl group, a nitrate group,
An alkyl group having 1 to 4 carbon atoms, an alkyl group having 1 to 4 main chain carbon atoms substituted with an acyloxy group, an alkyl group having 1 to 4 main chain carbon atoms substituted with a cyano group, a main chain substituted with an alkoxy group 0.1 to 3.5 parts by weight of one or more monoazo dyes represented by [alkyl group having 1 to 4 chain carbon atoms] and 1 to 15 parts by weight of at least one of an organic acid and a metal salt of an organic acid. An indicator composition for sterilization detection, comprising: