An o-phthalaldehyde disinfectant solution concentration detection indicator card and its preparation method

Abstract

The present invention relates to disinfection technology, and particularly to a quality control technology for o-phthalaldehyde disinfectant solution. A rapid detection indicator card impregnation composition for o-phthalaldehyde disinfectant solution, which comprises the following in mass percentages: stabilizer: 1% - 10%; chelating agent: 5% - 20%; neutralizing agent: 0.1% - 2%; chromogenic agent: 0.1% - 20%; chromogenic accelerator: 1% - 4%; the balance is pure water. After impregnating filter paper with the composition and drying it, it is pasted on white plastic paper with double-sided tape and compacted to form the rapid detection indicator card. The indicator card of the present invention has more stable, obvious and clear color development, rapid detection and more reliable results.

Description

Technical Field

[0001] The present invention relates to disinfection technology, and particularly to a quality control technology for o-phthalaldehyde disinfectant solution. Background Art

[0002] O-phthalaldehyde (OPA) was previously an important pharmaceutical and chemical intermediate. Since Alaf discovered in 1994 that it has a good disinfection effect for medical endoscopes, foreign research on the disinfection function of OPA has been very active. It has been developed into a new type of highly efficient disinfectant and has obtained the certification of the US FDA. Compared with glutaraldehyde, a disinfectant widely used in medical institutions currently, o-phthalaldehyde has a broader bactericidal spectrum, a lower use concentration, a shorter bactericidal time, less irritation, and weaker corrosion. In recent years, it has gradually replaced glutaraldehyde as a new generation of highly efficient medical disinfectant.

[0003] To ensure the high-level disinfection effect of o-phthalaldehyde, its effective concentration needs to be maintained above 3 g / L. Therefore, it is necessary to measure its concentration before use. Currently, the methods for measuring the concentration of o-phthalaldehyde include high-performance liquid chromatography, ultraviolet spectrophotometry, etc. These methods have complex testing processes and require professional equipment and operators. It is more convenient and fast to measure its effective concentration using a concentration indicating card.

[0004] In the prior art, many o-phthalaldehyde disinfectant solution concentration indicating cards and their preparation processes are disclosed. For example, Patent CN104215629A provides an aldehyde disinfectant concentration test paper, which is treated with a sulfite solution, an amino acid solution, and a stabilizer. The principle it adopts is that aldehydes react with amino acids to show yellow, but its formula is rough, and it does not disclose which concentration of aldehyde reagent is effective. Moreover, the color development time of the test paper is long, requiring 5 - 8 minutes. CN106970075B uses an o-phthalaldehyde concentration rapid detection test paper made of sodium bisulfite, methylene blue, a color developer, and a color development accelerator. When the color development accelerator is not added, the color development time requires 5 - 6 minutes. After adding the color development accelerator, the test paper still requires 90 seconds for color development, exceeding 1 minute. In addition, although in order to enhance the color development effect, a test paper with a light blue color is used, the final color development is blue-green, and the color development effect is still not obvious. CN107024473B discloses a preparation method for an o-phthalaldehyde disinfectant concentration detection test paper. The test paper mother liquor needs to be divided into liquid A and liquid B. Although a solid organic acid is added as a catalyst to accelerate the color development rate, the preparation process of the detection test paper is complex, the mother liquor has many components and high costs, and its color development effect is not obvious either: when the o-phthalaldehyde concentration exceeds 0.3%, it shows yellow, and when the concentration is less than 0.3%, it shows light yellow or does not show, and the color boundary is difficult to distinguish. Summary of the Invention

[0005] The present invention aims to solve the defects of the prior art and provides an o-phthalaldehyde disinfectant solution concentration detection indicator card and a preparation method thereof. The indicator card of the present invention has stable, obvious and clear color development, rapid detection and reliable results.

[0006] To achieve the above object, the present invention provides an o-phthalaldehyde disinfectant solution concentration detection indicator card impregnation composition, which is composed of the following substances in mass percentages:

[0007] Stabilizer: 1% - 10%;

[0008] Chelating agent: 5% - 20%;

[0009] Neutralizing agent: 0.1% - 2%;

[0010] Color developer: 0.1% - 20%;

[0011] Color development accelerator: 1% - 4%;

[0012] The balance is pure water.

[0013] Among them, the stabilizer is at least one of polyethylene glycol, polyvinylpyrrolidone, 1,3-butanediol, polypropylene copolymer, acrylate copolymer, hydroxypropyl cellulose, etc.

[0014] The chelating agent is at least one of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, citrate, pyrophosphate, thiosulfate, sulfite.

[0015] The neutralizing agent is at least one of carbonate, bicarbonate, phosphate, bisulfite, thiosulfate.

[0016] The color developer is an organic compound containing an imine or methylimine characteristic group.

[0017] Further, the color developer is at least one of urea, tryptophan, methionine, threonine, valine, lysine, histidine, leucine, isoleucine, alanine, phenylalanine, cystine, cysteine, arginine, glycine, serine, tyrosine, glutamic acid, aspartic acid, proline, hydroxyproline, citrulline, ornithine, tryptophan methyl ester, methionine methyl ester, threonine methyl ester, valine methyl ester, lysine ethyl ester, histidine methyl ester, leucine methyl ester, isoleucine ethyl ester, alanine methyl ester, phenylalanine methyl ester, cystine ethyl ester, cysteine methyl ester, arginine ethyl ester, glycine methyl ester, serine methyl ester, tyrosine methyl ester, glutamic acid methyl ester, aspartic acid methyl ester, proline ethyl ester, hydroxyproline methyl ester, citrulline methyl ester, ornithine ethyl ester, aromatic amine, aliphatic amine, etc.

[0018] The color development accelerator is at least one of dibasic hydrogen phosphate, ammonium carbonate, ammonium acetate.

[0019] Based on the fact that the aldehyde group of phthalaldehyde can undergo a condensation reaction with an amino group to form a yellow Schiff base, the neutralizer on the indicator card preferentially reacts with the phthalaldehyde adsorbed on the indicator card. When the concentration of phthalaldehyde is lower than the threshold value (3 g / L), all the phthalaldehyde is consumed and the reaction does not show color. When the concentration of phthalaldehyde is greater than or equal to the threshold value (3 g / L), the excess phthalaldehyde reacts with the amino group to show color. The reaction rate is fast and is not affected by environmental conditions such as the pH of the phthalaldehyde disinfectant solution, solution ions, and human operation. To accelerate the color development rate, at least one of phosphate, ammonium carbonate, and ammonium acetate with a buffering effect is selected in the present invention.

[0020] The present invention also provides a phthalaldehyde disinfectant solution concentration detection indicator card, which is impregnated with the above-mentioned impregnation composition.

[0021] The present invention also provides a preparation method of the above-mentioned phthalaldehyde disinfectant solution concentration detection indicator card, and the method includes: preparation of the impregnating solution and preparation of the indicator card. The preparation of the impregnating solution is to add a stabilizer, a complexing agent, a neutralizer, and a color developer into water in corresponding proportions according to mass percentages and stir evenly; the preparation of the indicator card is to soak filter paper in the impregnating solution, stir slowly, take out the filter paper after 3 - 5 minutes and place it on a glass plate; place the glass plate with the soaked filter paper in an oven at 40 - 80 °C for drying, and place the dried filter paper in a desiccator for static placement to obtain the indicator card. Among them, the drying time in the oven is 1 - 4 hours, and the static placement time in the desiccator is 0.5 - 1 hour.

[0022] The present invention also provides an application of the above-mentioned phthalaldehyde disinfectant solution concentration detection indicator card in detecting the concentration of phthalaldehyde disinfectant solution. When the mass concentration of the phthalaldehyde disinfectant solution is greater than or equal to 3 g / L, the color development is obvious brown, and when the mass concentration of the phthalaldehyde disinfectant solution is less than 3 g / L, there is no color development.

[0023] Under normal circumstances, after phthalaldehyde reacts with amino acid substances, it presents yellow on the test paper. If the concentration is unqualified, the test result will show light yellow or no color development, and the color development result is not obvious. Especially near the threshold value, it is difficult for the tester to quickly determine. In view of this problem, the inventor of the present invention surprisingly found that by adding the stabilizer and chelating agent described in the present invention, on the one hand, when the test paper prepared is used to detect the concentration of phthalaldehyde in the disinfectant solution, the dissolution of the chromogenic agent fixed on the test paper in the disinfectant solution can be reduced, thereby reducing the influence of the contact time between the test paper and the disinfectant solution and the color development time on the test result, as well as the pollution of the test indicator card to the phthalaldehyde disinfectant solution; on the other hand, by selecting the stabilizer and chelating agent in a specific ratio in the present invention, the color development result is significantly improved. When the concentration of phthalaldehyde is lower than the threshold value (0.3%), no color development occurs. When the concentration of phthalaldehyde is greater than or equal to the threshold value (0.3%), the test paper presents obvious brown within 30 s, and the brown gradually deepens with the extension of time.

[0024] The beneficial effects of the present invention are as follows:

[0025] 1. The concentration detection indicator card of the present invention can be used to detect the mass concentration range of phthalaldehyde disinfectant solution as 3 g / L - 6 g / L. The color development rate is fast. When the mass concentration of phthalaldehyde disinfectant solution is greater than or equal to 3 g / L, obvious brown appears within 30 s. When the mass concentration of phthalaldehyde disinfectant solution is less than 3 g / L, no color development occurs, and the color difference is obvious, which is easy to judge.

[0026] 2. The chromogenic agent in the present invention can stably adhere to the test paper, reducing the dissolution of amino groups in the disinfectant solution, thereby reducing the influence of the contact time between the test paper and the disinfectant solution and the color development time on the test result, as well as the pollution of the test indicator card to the phthalaldehyde disinfectant solution. The color development result is stable and clear.

[0027] 3. The formula in the present invention is simple, the cost is low, the production of the indicator card is simple and convenient, and the test method is also simple and stable, and it is less affected by the pH and concentration of the phthalaldehyde disinfectant solution and the operation of the tester (such as the time of dipping the disinfectant solution). Specific embodiments

[0028] All experimental methods used in the following examples are conventional methods unless otherwise specified. All materials, reagents, etc. used in the following examples can be obtained through commercial channels unless otherwise specified.

[0029] Example 1

[0030] Preparation of the impregnating solution:

[0031] Weigh 10 g of polyvinylpyrrolidone, 5 g of disodium ethylenediaminetetraacetate, 2 g of sodium bisulfite, 4 g of disodium hydrogen phosphate, and 4 g of urea, add pure water to 100 g, and stir evenly.

[0032] Preparation of the indicator card:

[0033] 1. Cut the filter paper into an appropriate size (about 20 cm * 15 cm).

[0034] 2. Put the cut filter paper into a beaker containing the impregnating solution, stir slowly during the soaking process, take out the filter paper after soaking for 5 minutes and place it on a glass plate, and note that there should be no bubbles between the filter paper and the glass plate.

[0035] 3. Place the glass plate with the soaked filter paper in an oven at 40 °C and dry for 4 hours, then take it out. Place the dried filter paper in a drying dish containing a desiccant and let it stand for about one hour to obtain the indicator card.

[0036] Example 2

[0037] Preparation of the impregnating solution:

[0038] Weigh 1 g of hydroxypropyl cellulose, 20 g of potassium pyrophosphate, 0.1 g of sodium bicarbonate, 2 g of ammonium acetate, and 20 g of glycine methyl ester, add pure water to 100 g, and stir evenly.

[0039] Preparation of the indicator card:

[0040] 1. Cut the filter paper into an appropriate size (about 20 cm * 15 cm).

[0041] 2. Put the cut filter paper into a beaker containing the impregnating solution, stir slowly during the soaking process, take out the filter paper after soaking for 5 minutes and place it on a glass plate, and note that there should be no bubbles between the filter paper and the glass plate.

[0042] 3. Place the glass plate with the soaked filter paper in an oven at 80 °C and dry for 1 hour, then take it out. Place the dried filter paper in a drying dish containing a desiccant and let it stand for about one hour to obtain the indicator card.

[0043] Example 3

[0044] Preparation of the impregnating solution:

[0045] Put 1 g of carboxymethyl cellulose, 7 g of ethylenediaminetetraacetic acid, 1 g of sodium bicarbonate, 0.1 g of p-aminobenzoic acid, and 1 g of ammonium carbonate, add pure water to 100 g, and stir evenly.

[0046] Preparation of the indicator card:

[0047] 1. Cut the filter paper into an appropriate size (about 20 cm * 15 cm).

[0048] 2. Put the cut filter paper into a beaker containing the impregnating solution, stir slowly during the soaking process, take out the filter paper after soaking for 3 minutes and place it on a glass plate, and note that there should be no bubbles between the filter paper and the glass plate.

[0049] 3. Place the glass plate with the soaked filter paper in an oven at 60 °C and dry it for 2 hours. Then take it out and place the dried filter paper in a drying dish with desiccant and let it stand for about 0.5 hours to obtain the indicator card.

[0050] Comparative Example 1

[0051] Polyvinylpyrrolidone is not added to the impregnating solution, and the rest is the same as in Example 1.

[0052] Comparative Example 2

[0053] Ethylenediamine is not added to the impregnating solution, and the rest is the same as in Example 2.

[0054] Discard the edge part (about 1 cm) of the filter paper after standing above. Immediately cut the remaining part into strips 8 mm wide. At the same time, cut 3M double-sided tape into strips 8 mm wide. Use this double-sided tape to paste the strip of filter paper on the white plastic paper. After slightly pressing it, continue to cut it into a square-shaped head indicator color block, which can be used to conveniently dip the disinfectant solution. Take an indicator card and immerse the indicator color block completely in the to-be-detected o-phthalaldehyde disinfectant solution. Take it out after about 3 seconds, with the color block side facing up, and place it horizontally to wait for color development.

[0055] Detect each example and comparative example, and the results are shown in Table 1.

[0056] Table 1:

[0057] Indicator card Detection concentration Contact time with disinfectant solution Color development time Color of color development Example 1 0.6％ 3s 28s Dark brown Example 2 0.2％ 3s 30s Colorless Example 3 0.3％ 3s 30s Brown Comparative example 1 0.6％ 3s 30s Yellow Comparative example 2 0.3％ 3s 30s Light yellow

[0058] The detected concentration of o-phthalaldehyde in Table 1 was measured using an Agilent 1260 Infinity II liquid chromatograph.

Claims

1. An impregnation composition for an effective concentration detection indicator card of o-phthalaldehyde disinfectant solution, characterized in that, It consists of substances with the following mass percentages as follows: Stabilizer: 1% - 10%; Chelating agent: 5% - 20%; Neutralizing agent: 0.1% - 2%; Chromogenic agent: 0.1% - 20%; Chromogenic accelerator: 1% - 4%; The balance is pure water; The chromogenic agent is an organic compound containing an imine or methylimine characteristic group; The stabilizer is at least one of polyethylene glycol, polyvinylpyrrolidone, 1,3 - butanediol, polypropylene copolymer, acrylate copolymer, hydroxypropyl cellulose; The chelating agent is at least one of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, citrate, pyrophosphate, thiosulfate, sulfite; The neutralizing agent is at least one of bisulfite, phosphate, carbonate, bicarbonate, thiosulfate; The chromogenic accelerator is at least one of dibasic hydrogen phosphate, ammonium carbonate, ammonium acetate.

2. The impregnating composition of the ortho-phthalaldehyde disinfectant solution effective concentration detection indicator card according to claim 1, characterized in that, The chromogenic agent is at least one of urea, tryptophan, methionine, threonine, valine, lysine, histidine, leucine, isoleucine, alanine, phenylalanine, cystine, cysteine, arginine, glycine, serine, tyrosine, glutamic acid, aspartic acid, proline, hydroxyproline, citrulline, ornithine, methyl tryptophan, methyl methionine, methyl threonine, methyl valine, ethyl lysine, methyl histidine, methyl leucine, ethyl isoleucine, methyl alanine, methyl phenylalanine, ethyl cystine, methyl cysteine, ethyl arginine, methyl glycine, methyl serine, methyl tyrosine, methyl glutamic acid, methyl aspartic acid, ethyl proline, methyl hydroxyproline, methyl citrulline, ethyl ornithine, aromatic amine, aliphatic amine.

3. An ortho-phthalaldehyde disinfectant solution effective concentration detection indicator card, characterized in that, The indicating card is impregnated with the impregnating composition according to any one of claims 1 - 2.

4. The preparation method of an o-phthalaldehyde disinfectant solution effective concentration detection indicator card as described in claim 3, characterized in that, The preparation method includes: Preparation of the impregnating solution: adding the stabilizer, complexing agent, neutralizing agent and chromogenic agent into water in corresponding proportions according to the mass percentage, and stirring evenly; and Preparation of the indicating card: Soaking the filter paper in the impregnating solution, stirring slowly, taking out the filter paper after 3 - 5 minutes and placing it on a glass plate; placing the glass plate with the soaked filter paper in an oven at 40 - 80°C for drying, and placing the dried filter paper in a desiccator for static placement to obtain the indicating card.

5. Use of an o-phthalaldehyde disinfectant effective concentration detection indicator card as described in claim 4 in detecting the concentration of o-phthalaldehyde disinfectant, characterized in that, When the concentration of o - phthalaldehyde disinfectant is greater than or equal to 3 g / L, it shows a brown color, and when the concentration of o - phthalaldehyde disinfectant is less than 3 g / L, it does not show a color.