A pressure steam sterilization five-category indicator ink formula and preparation method thereof

Abstract

The invention discloses a pressure steam sterilization five-category indicator ink formula and a preparation method thereof, which belongs to the technical field of steam sterilization, and is composed of the following raw materials in parts by weight: 40-50% of a connecting material, 20-40% of a high-temperature decomposition reaction factor, 0.1-2.0% of an indicator, 5-10% of a resistance adjustment factor, 10-20% of a diluent, and 10.0-20.0% of a waterproof oil, and the sum of the percentages of each raw material is 100%. The high-temperature decomposition reaction factor is a three-component compound of phenylalanine, aspartic acid, and an oxalic acid compound, and the waterproof oil is selected from emulsified paraffin oil. The beneficial effects of the invention are that it does not contain heavy metal lead, avoids lead exposure of hospital personnel, and provides a lead-free environment; the ink system is a water-based ink system without organic solvents, is green and environmentally friendly, and avoids environmental pollution; the indicator ink contains emulsified paraffin oil, which is waterproof oil, does not soak paper, does not stain, does not drop ink, does not flow and pollute medical equipment after sterilization, does not pollute sterilized items, and does not cause harm to the human body.

Description

Technical field:

[0001] The invention belongs to the technical field of steam sterilization, in particular to a pressure steam sterilization five-category indicator ink formula and a preparation method thereof. Background technology:

[0002] Adequate sterilization conditions are usually monitored by placing appropriate sterilization indicators in the sterilization room along with the products and / or items to be sterilized. Various sterilization indicators are known and used for this purpose, including chemical indicators and biological indicators. The advantage of chemical indicators is that they can be read immediately after the sterilization process is completed and can be traced at any time. They can be stored for a long time as proof of the sterilization compliance of hospital medical devices.

[0003] According to the national standard GB18282.1-2015 Sterilization chemical indicators for medical and health care products Sterilization quality monitoring Pressure steam chemical indicators classification:

[0004] Class 1 process indicators: used on the outside of individual packages to indicate whether the items have undergone the sterilization process, so as to distinguish sterilized or non-sterile items, such as sterilization indicator tapes and labels;

[0005] Category 2 specific test indicators: used for specific test operations of sterilizers, such as the BD test of pre-vacuum pressure steam sterilizers;

[0006] Class 3 single parameter indicators: used to test a single parameter in the sterilization process, such as time and temperature, and indicate exposure to a predetermined sterilization process variable, such as 134°C;

[0007] Category 4 multi-parameter indicators: used to test two or more parameters during the sterilization process, such as time and temperature, and indicate exposure to a predetermined sterilization process variable, such as a 134°C sterilization indicator card, 134°C, 4 min;

[0008] Class 5 comprehensive indicators: used to test all key parameters in the sterilization process, such as time, temperature and humidity. The key parameters of the sterilization process monitored are equal to or exceed the performance requirements of ISO11138 for biological indicators;

[0009] Class 6 Simulation Indicators: Used for testing of all critical parameters of the sterilization process, such as time, temperature and humidity, and are designed to match the critical parameters of a specific sterilization cycle.

[0010] According to the requirements of Part 3 of WS310.3 Hospital Sterilization Supply Center: Cleaning, Disinfection and Sterilization Effect Monitoring Standards, the Category V Sterilization Card is used for emergency sterilization of implants. A biological PCD containing a Category V chemical indicator is used for monitoring. If the chemical indicator is qualified, it can be released early. Biological monitoring requires cultivation for at least 30 minutes to issue results. This time cannot meet clinical needs. The Category V card has become the gold standard for early release of implants.

[0011] Patent CN208927160U introduces a five-category crawling card. A five-category crawling card is characterized in that it includes, from top to bottom, self-adhesive label paper, low-viscosity membrane, indicator sheet, chromatographic analysis filter paper, and substrate. The chromatographic analysis filter paper is arranged in the middle position of the substrate, and the indicator sheet is arranged in the middle position of the chromatographic analysis filter paper. The indicator sheet and the chromatographic analysis filter paper are clamped between the low-viscosity membrane and the substrate that are bonded to each other. The structure is complex to make. After the sterilization is completed, the crawling card reads the colored dye on the crawling card to reach the "pass" area, indicating that the sterilization package has reached the sterilization conditions. If the colored dye on the crawling card does not reach the "pass" area, it indicates that the sterilization package has not reached the sterilization conditions. At present, the five-category cards on the market are all crawling cards, and the indicator strip crawls in one direction or two directions. The errors caused by the complex production and manufacturing will affect the accuracy of the crawling of the indicator strip of the five-category crawling card, resulting in misjudgment of the sterilization results, which brings greater risks to infection control.

[0012] Patent CN202221191283.9 discloses a color-changing crawling chemical indicator card. A resistance-increasing indicating ink belt is provided on the card surface. The resistance-increasing indicating ink belt includes multiple sub-areas. The amount of catalyst contained in the ink in the previous sub-area is greater than the amount of catalyst contained in the ink in the latter sub-area according to a preset order. A dividing line is pre-provided on the card surface, and the dividing line is used to divide the multiple sub-areas of the resistance-increasing indicating ink belt into qualified areas and unqualified areas. Since the resistance-increasing indicating ink belt in this application includes multiple sub-areas with different color-changing abilities, after sterilization, it can be judged whether the sterilization is qualified according to whether the color-changing part reaches the qualified area. It is more intuitive and can effectively avoid the situation where users are prone to misjudgment of the sterilization effect when using the chemical indicator card. This crawling chemical indicator card brings difficulties to printing and is not easy to achieve mass production.

[0013] Regarding the Class V sterilization indicator of pressure steam, the Class V card has stronger resistance than the biological indicator and plays a key role in sterilization. The creeping card is limited in its large-scale clinical use due to its complex structure, high manufacturing cost and expensive price.

[0014] The steam sterilization indicator compositions currently used by many manufacturers include polyvalent metal compounds, such as lead carbonate and sulfur. When the color of the indicator is fully developed under steam sterilization conditions, the indicator turns brown or black. Due to environmental issues, lead compounds have been replaced by other polyvalent metal compounds. As described in U.S. Patent No. 6,200,000, it has been proposed to use bismuth to replace the lead in a given steam sterilization indicator composition. U.S. Patent No. 5,916,816 (Read), for example, includes: bismuth carbonate is used. Bismuth carbonate is an inorganic salt that is insoluble in water. The ink made of it uses an oily resin as a binder and a solvent oil such as xylene, butyl ester, and cyclohexanone as a diluent, which causes environmental pollution. Bismuth sulfide generated by bismuth carbonate and sulfide is insoluble in water, toxic, and weakly radioactive. Bismuth sulfide is a dark brown substance that cannot distinguish between qualified conditions and unqualified conditions within the gradient color development range required by the five-category card, and therefore cannot be used as a five-category card indicator ink.

[0015] Patent CN106634173A discloses a non-fading pressure steam sterilization chemical indicator ink and its preparation method and application. The ink is made of the following raw materials in weight percentage: 15-30% of a connecting material; 20-30% of a copper-containing compound; 5-10% of a sulfur-containing compound; 1-5% of a catalyst; and 40-50% of a solvent. The preparation method is as follows: first, dissolving the connecting material in a solvent, then sequentially adding the copper-containing compound, the sulfur-containing compound and the catalyst, stirring, and then grinding to obtain the product; when used, it is used for gravure, flexographic or screen printing to make an indicator card, an indicator label or an indicator tape in the form of a pressure steam sterilization chemical monitoring product, and can also be made into packaging materials. The invention can avoid the fading problem of conventional bismuth salt chemical indicator ink or lead salt chemical indicator ink during storage in a sterile room after discoloration; the preparation method and application are simple and easy.

[0016] The problem with this ink is that, according to the national standard inspection requirements: after the indicator is tested by a pressure steam resistance testing instrument at 121°C, 128°C, and 135°C for 20min, 6min, and 2min, the indicator reaches the standard black color; after a pressure steam sterilization process at 120°C, 127°C, and 134°C for 12.72min, 3.86min, and 1.272min, the color of the indicator is still black, with no color distinction, which does not comply with the relevant provisions of GB18282.1 for the five types of indicators. Despite the presence of a catalyst, the black gradient is not clearly distinguished, and false negatives occur during the instrument detection process.

[0017] At present, commonly used chemical indicator inks contain heavy metals such as lead ions, manganese ions or copper ions. Excessive intake of heavy metals can lead to heavy metal poisoning in the human body. CN201611181226.1 uses copper-containing compounds to prepare chemical indicator inks, avoiding the harm of lead. However, copper is a heavy metal and still poses a hazard after direct and large-scale contact with the human body.

[0018] Patent US2014 / 0370604A1 uses organic bismuth compounds, carbonates, sulfur sources and water to form an aqueous pressure steam sterilization chemical indicator composition, which is more environmentally friendly than solvent-based components. To date, most of the chemical indicators on the market use metal sulfide color-changing components, using metal compounds or metal salts, sulfur powder or organic sulfur as the sulfur source. After pressure steam sterilization, the two components react chemically with the assistance of other additives to generate darker metal sulfides. However, since this type of chemical indicator will be in direct contact with medical devices during use, the heavy metal components in the indicator will inevitably be contaminated with the wounds of surgical patients. Therefore, the use of indicators with this heavy metal formula has the risk of postoperative foreign body infection.

[0019] Regarding the Class V sterilization indicator of pressure steam, the Class V card has stronger resistance than the biological indicator and plays a key role in sterilization. The crawling card is limited in its large-scale clinical use due to its complex structure and the presence of heavy metals. Summary of the invention:

[0020] In order to solve the above problems and overcome the shortcomings of the prior art, the present invention provides a pressure steam sterilization five-category indicator ink, which is composed of the following raw materials in parts by weight: 40-50% of a connecting material, 20-40% of a high-temperature decomposition reaction factor, 0.1-2.0% of an indicator, 5-10% of a resistance adjustment factor, 10-20% of a diluent, and 10.0-20.0% of a waterproof oil, and the sum of the percentages of the various raw materials is 100%.

[0021] Furthermore, the binder is one or more of water-based acrylic resin, water-based polyurethane resin, and various derivatives of cellulose.

[0022] Furthermore, the high temperature decomposition reaction factors are a complex of phenylalanine, aspartic acid and oxalic acid compounds.

[0023] Furthermore, the resistance regulating factor is one or more of potassium aminosulfate and ammonium sulfate.

[0024] Furthermore, the indicator is one or more of methyl red, methyl orange, bromocresol blue and bromocresol green.

[0025] Furthermore, the diluent is selected from ethylene glycol monobutyl ether, n-propanol, ethanol, n-butanol, water and combinations thereof.

[0026] Furthermore, the waterproof oil is selected from emulsified paraffin oil.

[0027] A method for preparing a pressure steam sterilized five-category indicator ink comprises: adding a diluent, a connecting material, a high-temperature decomposition reaction factor, an indicator, a resistance regulating factor and a waterproof oil, mixing them evenly, stirring to obtain ink, printing and drying.

[0028] The third aspect of the present invention provides a method for using the five types of indicator inks for pressure steam sterilization, comprising:

[0029] Place the five-category card in the middle of the package of the item to be sterilized; perform the sterilization operation, and after sterilization is completed, take out the indicator card and observe the color change of the indicator part;

[0030] If the indicator part of this indicator card is the same color as or darker than the "standard green", it means that the sterilized items "have met the conditions required for sterilization"; if the indicator part is red or lighter than the "standard green", it means that the sterilized items "do not meet the sterilization requirements".

[0031] The indicator of the present invention can be used for flexible plate and screen printing. Five types of sterilization indicator cards can be printed with this indicator. Hospitals and users can visually observe the sterilization process of the equipment, ensure the monitoring of the sterilization quality of each sterilized object, and effectively prevent unqualified sterilized medical supplies or equipment from being used for patients.

[0032] Beneficial effects of the present invention

[0033] (1) The chemical indicator of the present invention does not contain heavy metal lead, thus avoiding lead exposure of hospital staff and providing a lead-free environment; the ink system is a water-based ink system without organic solvents, which is green and environmentally friendly and avoids environmental pollution;

[0034] (2) By adjusting the combination of ink components, it can meet the requirements of five types of sterilization indicators and reach the standards for hospital sterilization applications;

[0035] (3) The qualified rate of the chemical indicator of the present invention according to the relevant provisions of GB18282.1 for the five types of indicators is 100%. After high-temperature pressure steam sterilization, the color development effect is observed. The indicator ink contains waterproof oil emulsified paraffin oil. After sterilization, there is no paper bleeding, no staining, no ink loss, no ink flow and contamination of medical equipment, no contamination of sterilized items, and no harm to the human body;

[0036] (4) The preparation method of the present invention is simple, practical and easy to promote. Description of the drawings:

[0037] Attached Figure 1 It is the color development diagram of the ink of the indicator color block before the color development card of the present invention is sterilized;

[0038] Attached Figure 2It is the ink color development diagram of the sterilization qualified indicator color block after the color development card of the present invention is sterilized;

[0039] Attached Figure 3 It is the ink color development diagram of the sterilization unqualified indicating color block after the color development card of the present invention is sterilized;

[0040] Attached Figure 4 It is a linear equation diagram of temperature coefficients of five types of indicators of the present invention; Specific implementation method:

[0041] In the description of the present invention, specific details are only for a full understanding of the embodiments of the present invention. However, those skilled in the art should know that the implementation of the present invention is not limited to these details. In addition, well-known structures and functions are not described or demonstrated in detail to avoid blurring the key points of the embodiments of the present invention. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0042] Specific implementation of the present invention:

[0043] In order to better understand the present invention, a specific embodiment is used for illustration. It is worth emphasizing that the effect of this embodiment is not substantially different from the various embodiments within the protection scope of the present invention, including the respective reagents and the content ratio of the reagents, and all of them can achieve the effects described in the present invention and solve the above-mentioned problems. Other combinations are not described here.

[0044] To achieve the above objectives, the present invention is implemented through the following technical solutions:

[0045] A method for preparing five types of indicator ink sterilized by pressure steam, characterized in that it comprises the following steps:

[0046] Weigh 100g of raw materials for production, use 15-20g of diluent and 45-50g of connecting material, stir for 10 minutes, add 20-25g of high temperature decomposition reaction factor compound and stir for 15 minutes, add 0.1-0.15g of indicator and stir evenly, stir for 10 minutes, add 5.0-10g of resistance adjustment factor, stir for 10 minutes, add 10-12g of waterproof oil, stir and mix for 10 minutes, print, dry, and after color development inspection, cut and package.

[0047] The present invention will be further described in detail below in conjunction with specific embodiments. It should be noted that the specific embodiments are intended to explain the present invention rather than to limit it.

[0048] The sum of the percentages of the connecting material 40-50%, the high temperature decomposition reaction factor compound 20-40%, the resistance adjustment factor 5-10%, the indicator 0.1-2.0%, the diluent 10-20%, and the waterproof oil 10.0-20.0% is 100%;

[0049] The connecting material is one or more of water-based acrylic resin, water-based polyurethane resin, cellulose, and derivatives thereof, which plays a role in connecting the ink printing to the cardboard;

[0050] The high temperature decomposition reaction factor is a complex of three acids, namely, phenylalanine, aspartic acid and oxalic acid. The compound undergoes a carboxylic acid decomposition reaction under the optimum ratio (1:3:6-1:4:8) and with the participation of water vapor to generate carbon dioxide. Under the high temperature and high pressure conditions of (121-135° C.), the generated carbon dioxide is ensured to completely react with water vapor to generate carbonic acid. The reaction speed is adjusted by adding a resistance regulating factor mixture to meet the color development requirements at different times and temperatures. The diluent is ethylene glycol monobutyl ether, n-propanol, ethanol, n-butanol, water and a combination thereof. The diluent is mixed with a connecting material to form a uniform ink system.

[0051] The waterproof oil is emulsified paraffin oil. Transparent water-soluble emulsified paraffin oil with a high oil content is added to the ink and forms a waterproof film together with the binder. The waterproof film plays a waterproof role in two aspects. On the one hand, it prevents the ink from being wetted by water vapor under high temperature conditions, causing paper bleeding, ink loss, and contamination of sterilization equipment; in particular, the waterproof film can prevent the carbon dioxide generated after the decomposition of the composite acid from volatilizing, ensuring that the generated carbon dioxide completely reacts with water vapor to generate carbonic acid, thereby ensuring the thoroughness, adequacy and sensitivity of the reaction. Specific embodiment:

[0053] Example 1

[0054] Weigh 100g of raw materials for production, stir with 15g of ethanol, 5g of water and 35g of water-based acrylic resin for 10min; add 20g of composite acid in a ratio of 1:3:6 (2g of phenylalanine, 6g of aspartic acid, 12g of oxalic acid) and stir for 15min; add 0.2g of methyl red and 0.2g of bromocresol green, stir evenly, and stir for 10min; add 6.0g of resistance regulating factor potassium aminosulfate, stir for 10min; add 18.6g of waterproof oil emulsified paraffin oil, stir and mix for 10min; print and dry.

[0055] Example 2

[0056] Weigh 100g of raw materials for production, stir with 10g of ethylene glycol monobutyl ether, 10g of ethanol and 30g of water-based polyurethane resin for 10 minutes; add 25g of 1:4:7.5 ratio (2g of phenylalanine, 8g of aspartic acid, 15g of oxalic acid) and stir for 15 minutes; add 0.5g of methyl orange and 0.5g of bromocresol green, stir evenly, and stir for 10 minutes; add 10.0g of resistance regulating factor ammonium sulfate, stir and mix for 10 minutes; add 14.0g of waterproof oil emulsified paraffin oil, stir and mix for 10 minutes; print and dry.

[0057] Comparative Example 1

[0058] The difference from Example 1 is that a different resistance regulating factor, sodium hydroxide, is added to replace the existing resistance factor for resistance regulation;

[0059] Comparative Example 2

[0060] The difference from Example 1 is that other high temperature decomposition reaction factor acid tryptophan is added to replace oxalic acid;

[0061] Comparative Example 3

[0062] The difference from Example 1 is that no emulsified paraffin oil is added;

[0063] Comparative Example 4

[0064] The difference from Example 1 is that no emulsified paraffin oil is added, and the method disclosed in US3862824A is used in a cited manner, that is, the color cards prepared in the comparative example are sealed in nylon plastic envelopes, which are permeable to steam but prevent the material of the carrier from being washed away;

[0065] Test according to the requirements of five types of indicators in GB18282.1. The results are shown in Table 1: Color contrast under different temperatures and time, whether it is qualified;

[0066] Table 1: Color development comparison results of the embodiments and comparative examples at different temperatures and times

[0067]

[0068]

[0069] From the data in Table 1, we can see that:

[0070] (1) In Example 1 and Example 2, after the chemical indicator of the present invention was tested by a pressure steam resistance tester at 121°C, 128°C, and 135°C for 20 min, 6 min, and 2 min, the indicator reached the standard green color; after the pressure steam sterilization process at 120°C, 127°C, and 134°C for 12.72 min, 3.86 min, and 1.272 min, the color of the indicator was red and did not reach the standard green; the color differentiation was obvious; and it met the relevant provisions of the five types of indicators in GB18282.1;

[0071] After high-temperature pressure steam sterilization, observe the color development effect, and add emulsified oil to the indicator ink. When it comes into contact with water, it will not bleed paper, stain, or fall off. There is no ink flow to contaminate medical devices; it will not contaminate sterilized items and will not cause harm to the human body;

[0072] (2) Comparative Example 1 did not add other resistance regulating factors, and Comparative Example 2 used the high temperature decomposition reaction factor acid tryptophan instead of oxalic acid, but after sterilization, the purpose of color differentiation could not be achieved;

[0073] This is because only by adding the resistance factor and within the combination range specified by the high-temperature decomposition reaction factor (1:3:6-1:4:8) can the purpose of completely distinguishing the colors of the three groups of reactions by naked eye be achieved, and through the combination of the three acids, the colors can be distinguished to seconds. Any adjustment beyond this ratio will not achieve the desired result.

[0074] Comparative Example 3, in which no emulsified paraffin oil was added, produced paper bleeding, staining, and ink loss, and could not achieve the purpose of completely distinguishing the colors by observing the three groups of reactions with the naked eye;

[0075] No emulsified paraffin oil was added, and the method disclosed in US3862824A was used, that is, the color cards prepared in the comparative example were sealed in nylon plastic envelopes. These envelopes can permeate steam but prevent the carrier material from being washed away, which can alleviate the paper bleeding, dyeing, and ink loss to a certain extent, but cannot achieve the purpose of completely distinguishing the colors of the three groups of reactions by naked eye observation; this may be because the nylon plastic envelopes that can permeate steam cannot well prevent the volatilization of carbon dioxide generated after the decomposition of the composite acid, ensuring that the generated carbon dioxide completely reacts with water vapor to generate carbonic acid, ensuring the thoroughness and sensitivity of the reaction;

[0076] According to the temperature coefficient requirements of five types of indicators in GB18282.1: Figure 4 It can be seen that the linear equation is: y = -0.0714x + 9.9363; R 2 =0.9993;

[0077] The temperature coefficient is: 14.00 (the negative reciprocal of the slope of the calculation formula), which meets the requirements of the five types of indicators in GB18282.1, 6.00-14.00;

[0078] In summary:

[0079] (1) The chemical indicator of the present invention does not contain heavy metal lead, thus avoiding lead exposure of hospital staff and providing a lead-free environment; the ink system is a water-based ink system without organic solvents, which is green and environmentally friendly and avoids environmental pollution;

[0080] (2) By adjusting the combination of ink components, it can meet the requirements of five types of sterilization indicators and reach the standards for hospital sterilization applications;

[0081] (3) The qualified rate of the chemical indicator of the present invention according to the relevant provisions of GB18282.1 for the five types of indicators is 100%. After high-temperature pressure steam sterilization, the color development effect is observed. The indicator ink contains emulsified paraffin oil. The transparent water-soluble emulsified paraffin oil with a high oil content is added to the ink to form a waterproof film together with the connecting material. The waterproof film plays a waterproof role in two aspects. On the one hand, it prevents the ink from being wetted by water vapor under high temperature conditions, causing paper bleeding, ink loss, and contamination of sterilization equipment; in particular, the waterproof film can prevent the carbon dioxide generated after the decomposition of the composite acid from volatilizing, ensuring that the generated carbon dioxide completely reacts with water vapor to generate carbonic acid, thereby ensuring the thoroughness, adequacy and sensitivity of the reaction;

[0082] (4) The preparation method of the present invention is simple, practical and easy to promote.

Claims

1. A five-category indicator ink for pressure steam sterilization, comprising the following raw materials in parts by weight: Connecting material 40-50%, high temperature decomposition reaction factor 20-40%, indicator 0.1-2.0%, resistance adjustment factor 5-10%, diluent 10-20%, waterproof oil 10.0-20.0%, the sum of the percentages of each raw material is 100%; The high temperature decomposition reaction factors are three complexes of phenylalanine, aspartic acid and oxalic acid compounds; the weight ratio of the three complexes is (1:3:6-1:4:8); The resistance regulating factor is potassium aminosulfate or ammonium sulfate or a combination of the two; The indicator is one or a combination of two or more of methyl red, methyl orange, bromocresol blue and bromocresol green.

2. The five-category indicator ink for pressure steam sterilization according to claim 1, characterized in that The binder is one or more of water-based acrylic resin, water-based polyurethane resin, cellulose, and derivatives thereof.

3. The five-category indicator ink for pressure steam sterilization according to claim 1, characterized in that The diluent is one or a combination of two or more selected from ethylene glycol monobutyl ether, n-propanol, ethanol, n-butanol, and water.

4. The five-category indicator ink for pressure steam sterilization according to claim 1, characterized in that The waterproof oil is selected from emulsified paraffin oil.

5. The five-category indicator ink for pressure steam sterilization according to any one of claims 1 to 4, characterized in that The method for preparing five types of indicator inks sterilized by pressure steam comprises: adding diluent, connecting material, high temperature decomposition reaction factor, indicator, resistance regulating factor and waterproof oil, mixing evenly, stirring to obtain ink, printing and drying.

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