Low-temperature sterilization chemical indication ink as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of sterilization monitoring, and discloses low-temperature sterilization chemical indication ink as well as a preparation method and application thereof. The low-temperature sterilization chemical indication ink comprises the following components in parts by weight: 0.5-20 parts of a composite catalyst, 0.1-5 parts of a sterilization color-changing color developing agent, 0.2-5 parts of a stable color developing agent, 2-35 parts of an adhesive, 15-85 parts of a solvent and 0.1-10 parts of an auxiliary agent, the adhesive comprises shellac and ethyl cellulose in a mass ratio of (1-10): 1; the composite catalyst comprises a strong oxidizing catalyst and a Lewis acid catalyst. The indicating ink has excellent stability, adhesion, rapid sterilization responsiveness, high sensitivity and environmental protection property, is short in color changing time and uniform in color changing, can be used in the sterilization process of heat-sensitive medical apparatuses and instruments, medicine packaging materials, instant food and cold chain packaging, and has a wide application prospect. The method is suitable for a low-temperature hydrogen peroxide plasma sterilization or low-temperature ethylene oxide sterilization process, and a high-precision and high-reliability sterilization monitoring scheme is provided for the industries of medical treatment, medicine and food.

Description

Technical Field

[0001] The present invention relates to the technical field of sterilization monitoring and discloses a low-temperature sterilization chemical indicator ink and a preparation method and application thereof. Background Art

[0002] During the production of medical devices and materials, many raw materials and semi-finished products require sterilization to ensure the sterility of the final product. Low-temperature sterilization technology is widely used in medical institutions and medical device production, particularly to better protect heat-sensitive medical devices and materials, preventing deformation, damage, or performance degradation caused by high-temperature treatment while achieving the desired sterilization effect.

[0003] Low-temperature sterilization chemical indicator ink is a special ink that indicates whether the sterilization is successful by changing its color during the low-temperature sterilization process. It can judge the performance of the sterilization equipment and the reliability of the sterilization procedure by detecting the changes in the ink before and after sterilization. However, the low-temperature sterilization chemical indicator ink used in existing low-temperature sterilization technology has the following disadvantages: (1) Poor stability: Some indicators use a color change mechanism that triggers color changes through changes in pH value. They are easily affected by environmental humidity and pH, resulting in unstable color change effect and shelf life; (2) Slow reaction speed: Existing chemical indicator inks react slowly in low-temperature environments, resulting in a long sterilization process and affecting efficiency; (3) Insufficient sensitivity: Some indicator inks are insensitive to slight changes in low-temperature sterilization conditions and cannot accurately reflect the sterilization effect, increasing the risk of sterilization failure; (4) Limited scope of application: Existing indicator inks are mostly designed for specific sterilization conditions and are difficult to adapt to the needs of different sterilization scenarios; (5) Some indicator inks have high costs due to complex manufacturing processes or expensive raw materials, which increases sterilization costs.

[0004] Therefore, it is urgent to develop a low-temperature sterilization chemical indicator ink with rapid response, high sensitivity and excellent stability, which can accurately detect the sterilization process, improve the sterilization efficiency and meet the demand of low-temperature sterilization technology for high-performance indicator ink. Summary of the Invention

[0005] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a low-temperature sterilization chemical indicator ink and a preparation method and application thereof.

[0006] To achieve the above object, the technical solution adopted by the present invention is as follows:

[0007] In a first aspect, the present invention provides a low-temperature sterilization chemical indicator ink, comprising the following components in parts by weight: 0.5-20 parts of a composite catalyst, 0.1-5 parts of a sterilization color-changing developer, 0.2-5 parts of a stable color developer, 2-35 parts of an adhesive, 15-85 parts of a solvent, and 0.1-10 parts of an auxiliary agent; the adhesive comprises shellac and ethyl cellulose in a mass ratio of (1-10):1; the composite catalyst comprises a strong oxidizing catalyst and a Lewis acid catalyst.

[0008] The present invention is a low-temperature sterilized chemical indicator ink obtained by compounding a composite catalyst, a sterilization color-changing developer, a stable color developer, an adhesive, a solvent, and an auxiliary agent. The ink has excellent stability, adhesion, and rapid sterilization responsiveness, high sensitivity, and environmental protection. Wherein, the adhesive of the specific proportion of the present invention cooperates with other components to significantly improve the adhesion of the ink, ensure that it forms a firm attachment on different materials (plastic, metal, glass, etc.), and effectively prevents the color-changing layer from peeling off; and improves the stability of the ink, reduces the influence of humidity on the color-changing effect of the ink, so that the ink can maintain a stable color-changing performance under various environmental conditions; also cooperates with other components to improve the anti-aging performance of the ink, ensuring that its performance remains unchanged during long-term storage; and further improves the dispersibility of the developer in the ink, so that the color-changing effect is more uniform, avoids local color abnormalities caused by aggregation, and makes the indicator ink processing adaptability of the present invention excellent, and is suitable for a variety of printing processes (such as screen printing and inkjet printing). Secondly, the strong oxidizing catalyst in the composite catalyst of the present invention provides oxidizing power, while the Lewis acid catalyst promotes electron transfer. These two components work together to significantly enhance the reaction sensitivity of the indicator ink, making color change more rapid and significant, improving detection efficiency, enhancing color contrast, and improving the visual recognition of the sterilization status, ensuring stable color change under various conditions. Furthermore, the color change process of the low-temperature sterilization chemical indicator ink, formed by compounding the various components of the present invention, is unaffected by environmental factors and can intuitively display the sterilization status, providing a reliable sterilization monitoring method for industries such as medical and food.

[0009] As a preferred embodiment of the low-temperature sterilization chemical indicator ink of the present invention, the low-temperature sterilization chemical indicator ink includes the following components in parts by weight: 4-18 parts of a composite catalyst, 0.5-2.5 parts of a sterilization color-changing developer, 0.5-2 parts of a stable color developer, 24-35 parts of an adhesive, 20-80 parts of a solvent, and 2-5 parts of an additive.

[0010] As a preferred embodiment of the low-temperature sterilization chemical indicator ink of the present invention, the mass ratio of the shellac to the ethyl cellulose is (3-6):1.

[0011] Preferably, the mass ratio of shellac to ethyl cellulose is any one of 3:1, 4:1, 5:1, 6:1 or a range value between two of them.

[0012] As a preferred embodiment of the low-temperature sterilization chemical indicator ink of the present invention, the strong oxidizing catalyst includes at least one of ferric chloride, ferric bromide, copper chloride, and titanium tetrachloride; the Lewis acid catalyst includes at least one of boron trichloride, aluminum trichloride, aluminum tribromide, magnesium chloride, magnesium bromide, magnesium bromide hexahydrate, magnesium chloride hexahydrate, zinc chloride, and zinc bromide.

[0013] Preferably, the mass ratio of the strong oxidizing catalyst to the Lewis acid catalyst is (0.2-5):1.

[0014] As a preferred embodiment of the low-temperature sterilization chemical indicator ink of the present invention, the sterilization color-changing developer includes at least one of rhodamine B, bromophenol green, ferroin, bromophenol blue, and hydroquinone.

[0015] As a preferred embodiment of the low-temperature sterilization chemical indicator ink of the present invention, the stable color developer includes at least one of Permanent Yellow 12, Pigment Violet V19, Sudan Red, and Permanent Blue 10.

[0016] As a preferred embodiment of the low-temperature sterilization chemical indicator ink of the present invention, the solvent includes at least one of water, ethanol, ethylene glycol ethyl ether acetate, ethyl acetate, and isopropyl alcohol.

[0017] As a preferred embodiment of the low-temperature sterilization chemical indicator ink of the present invention, the auxiliary agents include an ultraviolet protective agent, a film-forming agent, a pH regulator, and a defoaming agent.

[0018] Preferably, the UV protectant includes a fluorescent whitening agent 52; the film-forming agent includes at least one of polyvinyl alcohol, polyvinyl pyrrolidone, and hydroxypropyl methylcellulose; and the pH regulator includes citric acid and / or sodium bicarbonate.

[0019] In a second aspect, the present invention provides applications of the low-temperature sterilization chemical indicator ink in the medical, pharmaceutical and food fields.

[0020] As a preferred embodiment of the low-temperature sterilized chemical indicator ink of the present invention, the low-temperature sterilization is low-temperature hydrogen peroxide plasma sterilization and / or low-temperature ethylene oxide sterilization.

[0021] The indicator ink of the present invention fully demonstrates its significant advantages in improving sterilization efficiency, extending the service life of the indicator ink and meeting environmental protection requirements due to its excellent stability, adhesion, rapid sterilization responsiveness, high sensitivity and environmental protection. It can be used in the sterilization process of heat-sensitive medical devices, pharmaceutical packaging materials, ready-to-eat foods and cold chain packaging. It is suitable for low-temperature hydrogen peroxide plasma sterilization and low-temperature ethylene oxide sterilization processes to solve the problem of performance degradation of traditional inks in low-temperature, high-humidity and strong oxidizing environments, and provide a high-precision and high-reliability sterilization monitoring solution for the medical, pharmaceutical and food industries.

[0022] In a third aspect, the present invention provides a method for preparing the low-temperature sterilization chemical indicator ink, comprising the following steps: mixing the adhesive and the solvent, adding the stable color developer, grinding, and then adding the sterilization color-changing developer, composite catalyst, and auxiliary agent and stirring to obtain the product.

[0023] The method for preparing the indicator ink of the present invention is simple, highly efficient, and requires no special conditions or materials. Furthermore, the ink is highly stable, and the color change before and after sterilization is unaffected by the external environment. The color change is highly stable and unaffected by environmental pH and humidity. Furthermore, the preparation process releases no toxic or hazardous substances, thus meeting environmental requirements.

[0024] Compared with the prior art, the beneficial effects of the present invention are as follows: First, the indicator ink made of the specific content components of the present invention has high stability. On the one hand, the color change effect is stable in extreme sterilization environments (ethylene oxide gas, hydrogen peroxide plasma), and is not affected by the external environment (such as temperature, humidity, pH, etc.), which can ensure the accuracy and reliability of the monitoring results; on the other hand, its dispersion performance is stable, which can effectively prevent the aggregation or stratification of the color-changing components, extend the shelf life of the ink, and is suitable for long-term storage and use, meeting the long-term stocking needs of the medical, food and other industries. Secondly, the indicator ink of the present invention has a short color change time and uniform color change, can quickly and accurately display the sterilization effect, and ensures consistent color changes without spots or unevenness while improving monitoring efficiency. At the same time, the indicator ink of the present invention has excellent adhesion properties, significantly improving the adhesion to a variety of sterilized packaging materials, ensuring that the ink coating can remain intact without swelling, cracking or peeling in extreme sterilization environments (ethylene oxide gas, hydrogen peroxide plasma). In addition, the indicator ink formula design of the present invention improves processing adaptability and is compatible with mainstream processes such as gravure printing, screen printing, and inkjet printing. It does not require special equipment modification, has a simple process, and is suitable for industrial production. DETAILED DESCRIPTION

[0025] To better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments. Those skilled in the art should understand that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0026] The following is an elaboration with reference to specific embodiments to illustrate the practical effects of the present invention.

[0027] Unless otherwise specified, the experimental methods used in the examples are conventional methods; the materials, reagents, equipment, etc. used are all available from commercial sources unless otherwise specified.

[0028] The raw materials used in the following examples and comparative examples are described below, but are not limited to these materials:

[0029] Table 1: Raw materials and manufacturers

[0030] raw material model factory synthetic shellac Chemically pure Sinopharm Ethyl cellulose EC-N4 Sinopharm Permanent Yellow Chemically pure Clariant Chemical Technology (Shanghai) Co., Ltd. Rhodamine B analytically pure Shanghai Aladdin Biochemical Technology Co., Ltd. Pigment Violet V19 analytically pure Shanghai Aladdin Biochemical Technology Co., Ltd. Basic Blue 6B analytically pure Shanghai Aladdin Biochemical Technology Co., Ltd. Sudan Red analytically pure Shanghai Aladdin Biochemical Technology Co., Ltd. Bromophenol green analytically pure Shanghai Aladdin Biochemical Technology Co., Ltd. polyvinyl acetate resin Chemically pure Sinopharm Fluorescent brightener 52 Chemically pure Sinopharm Polyvinyl alcohol film-forming agent Chemically pure Sinopharm defoaming agent silicone oil Sinopharm

[0031] Example 1: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0032] The indicator ink of this embodiment includes the following components in parts by weight: 25 parts of synthetic shellac, 5 parts of ethyl cellulose, 58.72 parts of anhydrous ethanol, 2 parts of permanent yellow, 0.5 parts of rhodamine B, 5 parts of FeBr3, 1 part of MgBr2·6H2O, 0.5 parts of fluorescent brightener 52, 2 parts of polyvinyl alcohol film-forming agent, 0.25 parts of citric acid and 0.03 parts of defoaming agent.

[0033] (1) Synthetic shellac and ethyl cellulose are completely dissolved in anhydrous ethanol under stirring to prepare an adhesive solution. Then, permanent yellow and ceramic zirconium beads with a particle size of 0.5-1.5 mm, which occupy 60%-85% of the volume of the grinding chamber, are added. The solution is ground at 3000 rpm in a horizontal sand mill for 30 minutes. The average particle size after grinding is 0.5 μm.

[0034] (2) Rhodamine B, FeBr3, MgBr2·6H2O, fluorescent brightener 52, polyvinyl alcohol film-forming agent, citric acid and defoaming agent are added respectively and stirred until completely dissolved and uniform to obtain the final indicator ink.

[0035] Example 2: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Blue to Red)

[0036] The indicator ink of this embodiment includes the following components in parts by weight: 25 parts of synthetic shellac, 5 parts of ethyl cellulose, 58.22 parts of anhydrous ethanol, 2 parts of pigment violet V19, 1 part of basic blue 6B, 5 parts of FeCl3, 1 part of MgCl2·6H2O, 0.5 parts of fluorescent brightener 52, 2 parts of polyvinyl alcohol film-forming agent, 0.25 parts of citric acid, and 0.03 parts of defoaming agent.

[0037] (1) Synthetic shellac and ethyl cellulose were completely dissolved in anhydrous ethanol under stirring to prepare an adhesive solution. Pigment Violet V19 and ceramic zirconium beads with a particle size of 0.5 mm to 1.5 mm, which occupied 60% to 85% of the volume of the grinding chamber, were then added. The mixture was ground at 3000 rpm for 30 minutes in a horizontal sand mill. The average particle size after grinding was 0.5 μm.

[0038] (2) Then add basic blue 6B, FeCl3, MgCl2·6H2O, fluorescent brightener 52, polyvinyl alcohol film-forming agent, citric acid and defoaming agent respectively and stir until they are completely dissolved and uniform to obtain the final indicator ink.

[0039] Example 3: Ethylene oxide sterilization indicator ink (blue to red)

[0040] The indicator ink of this embodiment includes the following components in parts by weight: 25 parts of synthetic shellac, 5 parts of ethyl cellulose, 48.72 parts of anhydrous ethanol, 2 parts of pigment violet V19, 1.5 parts of basic blue 6B, 5 parts of FeCl3, 12 parts of MgBr2·6H2O, 0.5 parts of fluorescent brightener 52, 2 parts of polyvinyl alcohol film-forming agent, 0.25 parts of citric acid, and 0.03 parts of defoaming agent.

[0041] (1) Synthetic shellac and ethyl cellulose were completely dissolved in anhydrous ethanol under stirring to prepare an adhesive solution. Pigment Violet V19 and ceramic zirconium beads with a particle size of 0.5 mm to 1.5 mm, which occupied 60% to 85% of the volume of the grinding chamber, were then added. The mixture was ground at 3000 rpm for 30 minutes in a horizontal sand mill. The average particle size after grinding was 0.5 μm.

[0042] (2) Then add basic blue 6B, FeCl3, MgBr2·6H2O, fluorescent brightener 52, polyvinyl alcohol film-forming agent, citric acid and defoaming agent respectively and stir until they are completely dissolved and uniform to obtain the final indicator ink.

[0043] Example 4: Ethylene oxide sterilization indicator ink (red to blue)

[0044] The indicator ink of this embodiment includes the following components in parts by weight: 20 parts of synthetic shellac, 4 parts of ethyl cellulose, 47.28 parts of anhydrous ethanol, 5 parts of propylene glycol, 0.5 parts of Sudan red, 2.5 parts of bromophenol green, 3 parts of FeCl3, 15 parts of MgBr2·6H2O, 0.5 parts of fluorescent whitening agent 52, 2 parts of polyvinyl alcohol film-forming agent, 0.25 parts of citric acid, and 0.03 parts of defoaming agent.

[0045] (1) Synthetic shellac and ethyl cellulose are completely dissolved in anhydrous ethanol under stirring to prepare an adhesive solution. Sudan red and ceramic zirconium beads with a particle size of 0.5 mm to 1.5 mm, which occupy 60% to 85% of the volume of the grinding chamber, are then added. The solution is ground at 3000 rpm in a horizontal sand mill for 30 minutes. The average particle size after grinding is 0.5 μm.

[0046] (2) Then, bromophenol green, FeCl3, MgBr2·6H2O, fluorescent brightener 52, polyvinyl alcohol film-forming agent, citric acid and defoaming agent were added and stirred until they were completely dissolved and uniformly dissolved to obtain the final indicator ink.

[0047] Example 5: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0048] The only difference between the indicator ink of this embodiment and that of Example 1 is that the indicator ink of this embodiment comprises the following components in parts by weight: 15 parts of synthetic shellac, 5 parts of ethyl cellulose, 20 parts of anhydrous ethanol, 0.5 parts of permanent yellow, 0.5 parts of rhodamine B, 3 parts of FeBr3, 1 part of MgBr2·6H2O, 0.5 parts of fluorescent brightener 52, 1 part of polyvinyl alcohol film-forming agent, 0.35 parts of citric acid, and 0.15 parts of defoaming agent.

[0049] Example 6: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0050] The only difference between the indicator ink of this embodiment and that of Example 1 is that the indicator ink of this embodiment comprises the following components in parts by weight: 30 parts of synthetic shellac, 5 parts of ethyl cellulose, 80 parts of anhydrous ethanol, 2 parts of permanent yellow, 0.5 parts of rhodamine B, 5 parts of FeBr3, 1 part of MgBr2·6H2O, 0.5 parts of fluorescent brightener 52, 2 parts of polyvinyl alcohol film-forming agent, 0.25 parts of citric acid, and 0.03 parts of defoaming agent.

[0051] Example 7: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0052] The only difference between the indicator ink of this embodiment and that of Example 1 is that the indicator ink of this embodiment comprises the following components in parts by weight: 15 parts of synthetic shellac, 1.5 parts of ethyl cellulose, 85 parts of anhydrous ethanol, 5 parts of permanent yellow, 5 parts of rhodamine B, 10 parts of FeBr3, 10 parts of MgBr2·6H2O, 6.5 parts of fluorescent brightener 52, 3 parts of polyvinyl alcohol film-forming agent, 0.45 parts of citric acid, and 0.05 parts of defoaming agent.

[0053] Example 8: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0054] The only difference between the indicator ink of this embodiment and that of Example 1 is that the indicator ink of this embodiment comprises the following components in parts by weight: 1 part of synthetic shellac, 1 part of ethyl cellulose, 15 parts of anhydrous ethanol, 0.2 part of permanent yellow, 0.1 part of rhodamine B, 0.4 part of FeBr3, 0.1 part of MgBr2·6H2O, 0.05 part of fluorescent brightener 52, 0.1 part of polyvinyl alcohol film-forming agent, 0.04 part of citric acid, and 0.01 part of defoaming agent.

[0055] Comparative Example 1: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0056] The only difference between the indicator ink of this comparative example and that of Example 1 is that the indicator ink of this comparative example does not include ethyl cellulose.

[0057] Comparative Example 2: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0058] The only difference between the indicator ink of this comparative example and that of Example 1 is that the indicator ink of this comparative example does not include synthetic shellac.

[0059] Comparative Example 3: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0060] The only difference between the indicator ink of this comparative example and Example 1 is that in the indicator ink of this comparative example, 25 parts of synthetic shellac and 5 parts of ethyl cellulose are replaced by 30 parts of polyvinyl acetate resin.

[0061] Comparative Example 4: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0062] The only difference between the indicator ink of this comparative example and Example 1 is that in the indicator ink of this comparative example, 5 parts of ethyl cellulose are replaced by 5 parts of synthetic shellac.

[0063] Comparative Example 5: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0064] The only difference between the indicator ink of this comparative example and Example 1 is that in the indicator ink of this comparative example, 25 parts of synthetic shellac are replaced by 25 parts of ethyl cellulose.

[0065] Comparative Example 6: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0066] The only difference between the indicator ink of this comparative example and that of Example 1 is that the indicator ink of this comparative example includes 30 parts of synthetic shellac and 2 parts of ethyl cellulose.

[0067] Comparative Example 7: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0068] The only difference between the indicator ink of this comparative example and that of Example 1 is that the indicator ink of this comparative example includes 10 parts of synthetic shellac and 20 parts of ethyl cellulose.

[0069] Comparative Example 8: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0070] The only difference between the indicator ink of this comparative example and that of Example 1 is that the indicator ink of this comparative example does not include FeBr 3 .

[0071] Comparative Example 9: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0072] The only difference between the indicator ink of this comparative example and that of Example 1 is that the indicator ink of this comparative example does not include MgBr2·6H2O.

[0073] Comparative Example 10: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0074] The only difference between the indicator ink of this comparative example and that of Example 1 is that in the indicator ink of this comparative example, 5 parts of FeBr 3 are replaced by 5 parts of MgBr 2 ·6H 2 O.

[0075] Comparative Example 11: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0076] The only difference between the indicator ink of this comparative example and that of Example 1 is that in the indicator ink of this comparative example, one part of MgBr2·6H2O is replaced by one part of FeBr3.

[0077] Comparative Example 12: Hydrogen Peroxide Plasma Sterilization Indicator Ink (Red to Yellow)

[0078] The indicator ink of this comparative example comprises: 25 parts of synthetic shellac, 5 parts of ethyl cellulose, 58.72 parts of anhydrous ethanol, 2 parts of permanent yellow, 0.5 parts of rhodamine B, 5 parts of FeBr3, 1 part of MgBr2·6H2O, 0.5 parts of fluorescent brightener 52, 2 parts of polyvinyl alcohol film-forming agent, 0.25 parts of citric acid and 0.03 parts of defoaming agent.

[0079] The synthetic shellac and ethyl cellulose were completely dissolved in anhydrous ethanol under stirring to prepare an adhesive solution, and then permanent yellow was added and mixed. Rhodamine B, FeBr3, MgBr2·6H2O, fluorescent brightener 52, polyvinyl alcohol film-forming agent, citric acid and defoaming agent were added respectively and stirred until completely dissolved and uniform to obtain the final indicator ink.

[0080] Test example: Performance test of indicator ink

[0081] The indicator inks of the examples and comparative examples were respectively coated on sterilized substrates to prepare indicator cards.

[0082] 1. Sterilization response accuracy performance test

[0083] Purpose: To evaluate whether the color change reaction of indicator ink in low temperature plasma sterilization environment is as expected.

[0084] Test Method: Indicator cards are placed in a standard sterilization load (low-temperature plasma sterilizer Sterrad100NX, V-Pro maX) and color changes are observed during the sterilization process. The color change (ΔE) is measured using a colorimeter (spectrophotometer) to ensure the discernibility and stability of the color change.

[0085] Test standard: The color change should meet the color contrast requirements of ISO 11140-1. Under the condition of qualified sterilization, the color change should reach the target color. Under the condition of unqualified sterilization, the color change should be significantly different from the target color, that is, the sterilization response accuracy is 100%.

[0086] Test conditions: H2O2 concentration of 2.3 mg / L, temperature of 50°C, exposure time of 6 minutes for sterilization compliance, i.e. the indicator card should reach the target color; exposure time of 7 seconds for sterilization failure, i.e. the indicator card color should be significantly different from the target color; H2O2 concentration of 2.3 mg / L, temperature of 27°C, exposure time of 10 minutes for sterilization compliance, i.e. the indicator card should reach the target color; exposure time of 10 seconds for sterilization failure, i.e. the indicator card color should be significantly different from the target color;

[0087] Test sample quantity: Test at least 10 indicator cards simultaneously to ensure data reliability; at least 3 independent sterilization cycles to verify the repeatability of the results.

[0088] 2. Physical performance test

[0089] (1) Adhesion test

[0090] Purpose: To evaluate the adhesion of ink on indicator cards and ensure that the color layer does not fall off before and after sterilization.

[0091] Test method: Based on ASTM D3359 (Coating Adhesion Test), perform a peel test using 3M tape (e.g., 3M600 Tape). Apply the tape to the surface of the indicator card, press for 5 seconds, then quickly remove it to observe if any ink is removed.

[0092] Test standard: Adhesion should reach level 4B or above (ASTM D3359 cross-cut test standard), and the color layer should not peel off over a large area, which will affect color identification after sterilization.

[0093] Test equipment: 3M 600 tape; grid knife (grid test).

[0094] Test conditions: room temperature (23±2°C), humidity 50±10% RH.

[0095] Test sample quantity: Test at least 5 indicator cards with the same indicator ink, and repeat the test 3 times for each indicator card.

[0096] (2) Wear resistance test

[0097] Purpose: To test the friction resistance of indicator cards and ensure that the indicator layer is not easily damaged before and after sterilization.

[0098] Test Method: Tested in accordance with ISO 15184 (pencil hardness test) or ASTM D5264 (paper abrasion test) using a Taber 5135 abrasion tester. Rub the paper back and forth 50 times with a pressure of 500g, observing whether the color layer falls off or changes color.

[0099] Test standard: The color layer is still clearly visible after 50 times of friction, without obvious peeling.

[0100] Test instrument: Taber 5135 abrasion tester; 500g load block.

[0101] Test conditions: 23±2℃, 50±10%RH.

[0102] Test sample quantity: Test at least 5 indicator cards with the same indicator ink, and test each card 3 times.

[0103] 3. Stability performance test

[0104] (1) Accelerated aging test

[0105] Purpose: To evaluate the stability of indicator inks during long-term storage.

[0106] Test method: According to ASTM F1980 (Accelerated Aging Test for Medical Products), high-temperature accelerated aging (60°C, 60% RH, 4 weeks) was performed in a constant temperature and humidity chamber. The color change of the indicator card before and after aging was compared, and the ΔE value was measured.

[0107] Test standard: The color change ΔE value should be less than 2 (to ensure color stability during long-term storage).

[0108] Test instruments: constant temperature and humidity test chamber; spectrophotometer

[0109] Test conditions: Temperature: 60°C; Humidity: 60% RH; Time: 4 weeks (equivalent to 1 year of natural aging).

[0110] Test sample quantity: Test at least 10 indicator cards with the same indicator ink, and test each card 3 times.

[0111] (2) Light stability test

[0112] Purpose: To evaluate the light resistance of indicator inks and ensure that there is no color change caused by light during storage and transportation.

[0113] Test method: According to ISO 105-B02 (color fastness to light test), use a xenon arc tester (Xenon Arc Tester) and set the irradiation energy (such as 0.75W / m 2 ), irradiate continuously for 24 hours, and record the color change.

[0114] Test standard: The color change ΔE value should be less than 2, and the indicator layer should not change color prematurely due to light exposure.

[0115] Testing instrument: Xenon lamp light resistance testing machine.

[0116] Test conditions: Light intensity: 0.75W / m 2 , time: 24 hours.

[0117] Test sample size: Test at least 10 indicator cards with the same indicator ink, and measure each card 3 times.

[0118] Table 2: Performance test results of indicator inks of the present invention and comparative examples

[0119]

[0120]

[0121] It can be seen from the data in Table 1 that: compared with Example 1, the indicator inks of Comparative Examples 1-7 do not use a specific ratio of synthetic shellac and ethyl cellulose or the mass ratio is not (1-10):1, so that the overall performance of the indicator inks of Comparative Examples 1-7 is worse than that of the indicator ink of the present invention; the indicator inks of Comparative Examples 8, 9 and Comparative Examples 10, 11 use a single catalyst, resulting in poor sterilization response accuracy and stability of the indicator inks; the indicator ink of Comparative Example 12 does not use a specific grinding process, resulting in poor adhesion and stability of the indicator ink.

[0122] Thus, first, the indicator ink made of the specific content component of the present invention has high stability. On the one hand, the color change effect is stable in extreme sterilization environments (ethylene oxide gas, hydrogen peroxide plasma), and is not disturbed by the external environment (such as temperature, humidity, pH, etc.), which can ensure the accuracy and reliability of the monitoring results; on the other hand, its dispersion performance is stable, which can effectively prevent the color-changing components from aggregating or stratifying, prolong the shelf life of the ink, and is suitable for long-term storage and use, meeting the long-term stocking needs of industries such as medical care and food. Secondly, the indicator ink of the present invention has a short color change time and uniform color change, which can quickly and accurately display the sterilization effect, improve the monitoring efficiency, and ensure that the color change is consistent without spots or unevenness. At the same time, the indicator ink of the present invention has excellent adhesion performance, significantly improves the adhesion to a variety of sterilization packaging materials, and ensures that the ink coating can remain intact under extreme sterilization environments (ethylene oxide gas, hydrogen peroxide plasma) without swelling, cracking or peeling. In addition, the indicator ink formula design of the present invention improves processing adaptability, is compatible with mainstream processes such as gravure printing, screen printing, and inkjet printing, does not require special equipment modification, and is simple in process and suitable for industrial production.

[0123] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A low-temperature sterilization chemical indicator ink, characterized in that: The invention comprises the following components in parts by weight: 0.5-20 parts of a composite catalyst, 0.1-5 parts of a sterilizing color-changing developer, 0.2-5 parts of a stable color developer, 2-35 parts of an adhesive, 15-85 parts of a solvent, and 0.1-10 parts of an auxiliary agent; the adhesive comprises shellac and ethyl cellulose in a mass ratio of (1-10):1; and the composite catalyst comprises a strong oxidizing catalyst and a Lewis acid catalyst.

2. The low-temperature sterilization chemical indicator ink according to claim 1, characterized in that: The invention comprises the following components in parts by weight: 4-18 parts of composite catalyst, 0.5-2.5 parts of sterilization color-changing developer, 0.5-2 parts of stable color developer, 24-35 parts of adhesive, 20-80 parts of solvent and 2-5 parts of auxiliary agent.

3. The low-temperature sterilization chemical indicator ink according to claim 1, characterized in that: The mass ratio of the shellac to the ethyl cellulose is (3-6):

1.

4. The low-temperature sterilization chemical indicator ink according to claim 3, characterized in that: The mass ratio of the shellac to the ethyl cellulose is 5:

1.

5. The low-temperature sterilization chemical indicator ink according to claim 1, characterized in that: The strong oxidizing catalyst includes at least one of ferric chloride, ferric bromide, copper chloride, and titanium tetrachloride; the Lewis acid catalyst includes at least one of boron trichloride, aluminum trichloride, aluminum tribromide, magnesium chloride, magnesium bromide, magnesium bromide hexahydrate, magnesium chloride hexahydrate, zinc chloride, and zinc bromide.

6. The low-temperature sterilization chemical indicator ink according to claim 1, characterized in that: The sterilization color-changing color developer includes at least one of rhodamine B, bromophenol green, ferroin, bromophenol blue, and hydroquinone.

7. The low-temperature sterilization chemical indicator ink according to claim 1, characterized in that: The stable color developer includes at least one of Permanent Yellow 12, Pigment Violet V19, Sudan Red, and Permanent Blue 10.

8. The low-temperature sterilization chemical indicator ink according to claim 1, characterized in that: The solvent includes at least one of water, ethanol, ethylene glycol ethyl ether acetate, ethyl acetate, and isopropyl alcohol.

9. Use of the low-temperature sterilization chemical indicator ink according to any one of claims 1 to 8 in the medical, pharmaceutical and food fields.

10. The method for preparing the low-temperature sterilization chemical indicator ink according to any one of claims 1 to 8, characterized in that: The following steps are involved: The adhesive and the solvent are mixed, the stable color developer is added, and the mixture is ground. Then, the sterilization color-changing developer, the composite catalyst, and the auxiliary agent are added and stirred to obtain the product.

Images