A salt-tolerant povidone-iodine concentrate and a method of making the same
By using a complexation reaction between dispersants such as alkyl benzyl polyoxyethylene ether and potassium iodate stabilizer, the problem of poor solubility of high-concentration povidone-iodine under low pH and high salinity conditions was solved, achieving high stability and biosafety of povidone-iodine concentrate.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- 成都科宏达科技有限公司
- Filing Date
- 2024-01-25
- Publication Date
- 2026-07-21
AI Technical Summary
High-concentration povidone-iodine concentrate has poor solubility and is prone to aggregation under low pH and high salinity conditions. Existing surfactants have poor solubilizing effect and poor biodegradability.
Alkyl benzyl polyoxyethylene ether or alkyl benzyl polyoxyethylene polyoxypropylene ether was used as a dispersant, and potassium iodate was used as a stabilizer. The solubility and stability of povidone-iodine were improved through a complexation reaction. Ethanol and other solvents were used and the pH value was adjusted to prepare a salt-resistant povidone-iodine concentrate.
It improves the solubility and stability of high-concentration povidone-iodine, avoids agglomeration, enhances biosafety, and has a simple preparation method with no byproducts.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of disinfection technology, specifically to a salt-resistant and highly stable povidone-iodine concentrate and its preparation method. Background Technology
[0002] Povidone-iodine is a loose complex composed of iodine and a polymer carrier. Povidone acts as a carrier and a solubilizer. It is a broad-spectrum and powerful bactericidal disinfectant with strong killing effects on viruses, bacteria, fungi, and mold spores. It is widely used in the medical, animal husbandry and other industries.
[0003] Povidone-iodine is typically produced at low concentrations, usually between 0.7% and 10%, with an effective iodine concentration of 0.0018% to 0.024%. The low effective iodine concentration, combined with the presence of other surfactants as co-solvents, contributes to the solution's stability. However, high-concentration povidone-iodine or concentrated povidone-iodine solutions are less stable during long-term storage due to their higher povidone-iodine content. Iodine content and pH decrease rapidly, and concentrated povidone-iodine solutions exhibit poor solubility and are prone to aggregation under low pH and high salinity conditions.
[0004] Existing solutions to this technical problem generally employ nonylphenol polyoxyethylene ether, benzylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, alkyl polyglycosides, N-alkyl glucamide, fatty acid methyl ester ethoxylated compounds, etc. Nonylphenol and benzylphenol polyoxyethylene ethers have good solubilizing effects, but poor biodegradability and environmental irritation. While fatty alcohol polyoxyethylene ethers, isomeric alcohol polyoxyethylene ethers, and alkyl polyglycosides have good biodegradability, their solubilizing effect in povidone-iodine concentrate (10% available iodine) is still poor, and aggregation occurs. Usually, a combination of several surfactants is needed to achieve a better effect. Summary of the Invention
[0005] To address the aforementioned problems, this invention proposes a salt-resistant povidone-iodine concentrate that can increase the complexation between polyvinylpyrrolidone and iodine, thereby improving the solubility and stability of povidone-iodine at high concentrations.
[0006] To achieve the above objectives, the present invention is implemented through the following technical solution:
[0007] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight of 100: 15-30 parts polyvinylpyrrolidone, 10-15 parts iodine, 25-35 parts solvent, 0.5-5 parts dispersant, 0-1 part stabilizer, 0.5-3 parts cosolvent, 0-5 parts pH adjuster, and the balance being water.
[0008] The dispersant is an alkyl benzyl polyether.
[0009] Furthermore, the dispersant includes any one or more of alkyl benzyl polyoxyethylene ether and alkyl benzyl polyoxyethylene polyoxypropylene ether.
[0010] Furthermore, the alkyl group in the alkyl benzyl polyoxyethylene ether is a straight-chain or branched alkyl group of C10-C22.
[0011] Furthermore, the alkyl group in the alkylbenzyl polyoxyethylene polyoxypropylene ether is a straight-chain or branched alkyl group of C10-C22.
[0012] Furthermore, the solvent includes one or more of ethanol, ethylene glycol, n-propanol, isopropanol, propylene glycol, and glycerol.
[0013] Furthermore, the stabilizer is potassium iodate.
[0014] Furthermore, the co-solvent is potassium iodide.
[0015] Furthermore, the pH adjuster includes one or more of sodium hydroxide, citric acid and sodium citrate, phosphoric acid and sodium dihydrogen phosphate.
[0016] This invention also discloses a method for preparing a salt-tolerant povidone-iodine concentrate, characterized by comprising the following steps:
[0017] (1) Dissolve polyvinylpyrrolidone in a solvent, then add iodine and co-solvent, stir and heat to 40-60℃ for complexation reaction for 2-5 hours;
[0018] (2) After the reaction is complete, add a pH adjuster to adjust the pH of the solution to 3-6, then add a dispersant and a stabilizer, add water to 100 parts, and stir for 0.5-1h to obtain the solution.
[0019] The beneficial effects of the present invention, namely, salt-resistant povidone-iodine concentrate and its preparation method, are as follows:
[0020] (1) In this invention, alkyl benzyl polyether is introduced during the complexation of povidone-iodine. The addition of long-chain alkyl groups on one side of the benzene ring in the molecular structure of alkyl benzyl polyether increases the lipophilicity of alkyl benzyl polyether. At the same time, when a polyether with a specific number of EO is added, the hydrophilic and lipophilic groups of the polyether are balanced as the number of EO increases, and the free energy of the molecules to form micelles decreases. Therefore, its CMC decreases, surface activity is enhanced, and emulsification ability is increased. This allows povidone-iodine to be rapidly dispersed in water without agglomeration, thereby increasing the solubility and stability of high-concentration povidone-iodine concentrate.
[0021] (2) The surfactant alkylbenzyl polyether added in this invention replaces the phenolic oxygen structure with a benzyl oxygen structure, thereby avoiding the biodegradability and reproductive toxicity caused by the phenolic oxygen structure and exhibiting good biosafety. At the same time, the preparation method of this product is simple, with no byproducts such as uncomplexed iodine or organic solvents generated, and the raw material utilization rate is high. Detailed Implementation
[0022] To enable those skilled in the art to better understand the present invention, the technical solution of the present invention will be clearly and completely described below with reference to embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0023] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight of 100: 15-30 parts polyvinylpyrrolidone, 10-15 parts iodine, 25-35 parts solvent, 0.5-5 parts dispersant, 0-1 part stabilizer, 0.5-3 parts cosolvent, 0-5 parts pH adjuster, and the balance being water.
[0024] The dispersant is an alkyl benzyl polyether.
[0025] It should be further noted that the dispersant includes any one or more of alkyl benzyl polyoxyethylene ether and alkyl benzyl polyoxyethylene polyoxypropylene ether.
[0026] As one example, the dispersant is an alkylbenzyl polyoxyethylene ether, wherein the alkyl group is a straight-chain or branched alkyl group of C10-C22, and the polyoxyethylene ether is a polyoxyethylene ether with an EO number of 5-11.
[0027] Preferably, the dispersant is alkylbenzyl polyoxyethylene ether, wherein the alkyl group is a straight-chain or branched alkyl group of C10-C16.
[0028] Specifically, the alkylbenzyl polyoxyethylene ether is any one or more of nonylbenzyl polyoxyethylene ether, dodecylbenzyl polyoxyethylene ether, tetradecylbenzyl polyoxyethylene ether, and hexadecylbenzyl polyoxyethylene ether.
[0029] In another embodiment, the dispersant is alkylbenzyl polyoxyethylene polyoxypropylene ether.
[0030] Preferably, the dispersant is alkylbenzyl polyoxyethylene polyoxypropylene ether, wherein the alkyl group is a straight-chain or branched alkyl group of C10-C16. The polyoxyethylene ether has an EO number of 5-11, and the polyoxypropylene has a PO number of 5-11.
[0031] Specifically, the alkylbenzyl polyoxyethylene polyoxypropylene ether is any one or more of nonylbenzyl polyoxyethylene polyoxypropylene ether, dodecylbenzyl polyoxyethylene polyoxypropylene ether, tetradecylbenzyl polyoxyethylene polyoxypropylene ether, and hexadecylbenzyl polyoxyethylene polyoxypropylene ether.
[0032] The preparation method of benzyl polyoxyethylene ether is as follows: alkyl benzyl alcohol, ethylene oxide, and sodium methoxide catalyst are placed in a high-pressure reactor. The alkyl benzyl alcohol and ethylene oxide are mixed in a molar ratio of 1:5-11. The amount of sodium methoxide added is 0.1%-5% of the mass of alkyl benzyl alcohol. The temperature in the high-pressure reactor is maintained at 120-140℃ and the reaction is carried out for 30 hours. After the reaction is completed, the mixture is cooled, washed with deionized water, the upper layer is extracted with petroleum ether, and the petroleum ether is removed by rotary evaporation to obtain benzyl polyoxyethylene ether.
[0033] The specific reaction formula is as follows:
[0034] The preparation method of benzyl polyoxyethylene polyoxypropylene ether is as follows: alkyl benzyl alcohol, ethylene oxide, propylene oxide, and sodium methoxide catalyst are placed in a high-pressure reactor. The ratio of alkyl benzyl alcohol, ethylene oxide, and propylene oxide is 1:2-10:2-10. The amount of sodium methoxide added is 0.1%-5% of the mass of alkyl benzyl alcohol. The temperature in the high-pressure reactor is maintained at 120-140℃, and the reaction is carried out for 30 hours. After the reaction is completed, the mixture is cooled, washed with deionized water, the upper layer is extracted with petroleum ether, and the petroleum ether is removed by rotary evaporation to obtain benzyl polyoxyethylene polyoxypropylene ether.
[0035] It should be further noted that the solvent includes one or more of ethanol, ethylene glycol, n-propanol, isopropanol, propylene glycol, and glycerol. Ethanol is preferred in this invention.
[0036] It should be further noted that the stabilizer is potassium iodate.
[0037] It should be further noted that the co-solvent is potassium iodide.
[0038] It should be further noted that pH adjusters include one or more of sodium hydroxide, citric acid and sodium citrate, phosphoric acid and sodium dihydrogen phosphate.
[0039] Method Example 1
[0040] A method for preparing a salt-resistant povidone-iodine concentrate includes the following steps:
[0041] (1) Dissolve polyvinylpyrrolidone in a solvent, then add iodine and co-solvent, stir and heat to 40°C for complexation reaction for 5 hours;
[0042] (2) After the reaction is complete, add pH adjuster to adjust the pH of the solution to 3, then add dispersant and stabilizer, add water to 100 parts, and stir for 1 hour to obtain the solution.
[0043] Method Example 2
[0044] A method for preparing a salt-resistant povidone-iodine concentrate includes the following steps:
[0045] (1) Dissolve polyvinylpyrrolidone in a solvent, then add iodine and co-solvent, stir and heat to 50°C for complexation reaction for 3 hours;
[0046] (2) After the reaction is complete, add pH adjuster to adjust the pH of the solution to 4, then add dispersant and stabilizer, add water to 100 parts, and stir for 1 hour to obtain the solution.
[0047] Method Example 3
[0048] A method for preparing a salt-resistant povidone-iodine concentrate includes the following steps:
[0049] (1) Dissolve polyvinylpyrrolidone in a solvent, then add iodine and co-solvent, stir and heat to 60°C for complexation reaction for 2 hours;
[0050] (2) After the reaction is complete, add a pH adjuster to adjust the pH of the solution to 6, then add a dispersant and a stabilizer, add water to make up to 100 parts, and stir for 1 hour to obtain the solution.
[0051] Method Example 4
[0052] A method for preparing a salt-resistant povidone-iodine concentrate includes the following steps:
[0053] (1) Dissolve polyvinylpyrrolidone in a solvent, then add iodine and a co-solvent, stir and heat to 45°C for a complexation reaction for 2.5 h;
[0054] (2) After the reaction is complete, add pH adjuster to adjust the pH of the solution to 3, then add dispersant and stabilizer, add water to 100 parts, and stir for 1 hour to obtain the solution.
[0055] Example 1
[0056] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dodecyl benzyl 9 polyoxyethylene ether dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water;
[0057] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0058] Example 2
[0059] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 19 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethylene glycol, 1 part dodecyl benzyl 11 polyoxyethylene ether dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water;
[0060] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0061] Example 3
[0062] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 19 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts isopropanol, 3 parts dodecyl benzyl 10 polyoxyethylene ether (dispersant), 0.2 parts potassium iodate (stabilizer), 0.9 parts potassium iodide (co-solvent), and the balance being water.
[0063] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0064] Example 4
[0065] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 17 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts propylene glycol, 2 parts dodecyl benzyl 5 polyoxyethylene ether dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water.
[0066] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0067] Example 5
[0068] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 30 parts polyvinylpyrrolidone, 15 parts iodine, 35 parts glycerol, 5 parts dodecyl benzyl 7 polyoxyethylene ether (dispersant), 1 part potassium iodate (stabilizer), 3 parts potassium iodide (co-solvent), and the remainder is water.
[0069] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0070] Example 6
[0071] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 25 parts polyvinylpyrrolidone, 15 parts iodine, 30 parts ethanol, 5 parts dodecyl benzyl 11 polyoxyethylene ether dispersant, 1 part potassium iodate stabilizer, 3 parts potassium iodide cosolvent, and the remainder is water.
[0072] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0073] Example 7
[0074] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 12 parts iodine, 30 parts ethanol, 2 parts dodecyl benzyl 11 polyoxyethylene ether dispersant, 0.5 parts potassium iodate stabilizer, 2 parts potassium iodide cosolvent, and the balance being water.
[0075] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0076] Example 8
[0077] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight of 100: 15 parts polyvinylpyrrolidone, 10 parts iodine, 25 parts ethanol, 1 part dodecyl benzyl 7 polyoxyethylene ether dispersant, 0.2 parts potassium iodate stabilizer, 2 parts potassium iodide cosolvent, and the balance being water.
[0078] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0079] Example 9
[0080] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts nonylalkylbenzyl 11 polyoxyethylene ether (dispersant), 0.2 parts potassium iodate (stabilizer), 0.9 parts potassium iodide (co-solvent), and the balance being water.
[0081] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0082] Example 10
[0083] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant tetradecylbenzyl 7 polyoxyethylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water.
[0084] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0085] Example 11
[0086] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant cetylbenzyl 5 polyoxyethylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water;
[0087] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0088] Example 12
[0089] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts nonylbenzyl 5 polyoxyethylene-5 polyoxypropylene ether dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water;
[0090] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0091] Example 13
[0092] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dodecyl benzyl 5 polyoxyethylene-7 polyoxypropylene ether dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water;
[0093] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0094] Example 14
[0095] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dodecyl benzyl 5 polyoxyethylene-5 polyoxypropylene ether dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water.
[0096] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0097] Example 15
[0098] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant dodecyl benzyl 7 polyoxyethylene-5 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts co-solvent potassium iodide, and the balance being water;
[0099] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0100] Example 16
[0101] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant dodecyl benzyl 7 polyoxyethylene-7 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water;
[0102] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0103] Example 17
[0104] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant tetradecylbenzyl 7 polyoxyethylene-7 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water;
[0105] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0106] Example 18
[0107] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant tetradecylbenzyl 5 polyoxyethylene-5 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water.
[0108] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0109] Example 19
[0110] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant tetradecylbenzyl 7 polyoxyethylene-7 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water;
[0111] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0112] Example 20
[0113] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant cetylbenzyl 5 polyoxyethylene-7 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water;
[0114] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0115] Example 21
[0116] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant cetylbenzyl 5 polyoxyethylene-5 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water;
[0117] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0118] Example 22
[0119] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant cetylbenzyl 7 polyoxyethylene-7 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water;
[0120] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0121] Example 23
[0122] A salt-resistant povidone-iodine concentrate comprises the following components, in parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant cetylbenzyl 9 polyoxyethylene-5 polyoxypropylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts cosolvent potassium iodide, and the balance being water;
[0123] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0124] Comparative Example 1
[0125] A povidone-iodine solution, in 100 parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts nonylphenol polyoxyethylene ether dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water;
[0126] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0127] Comparative Example 2
[0128] A povidone-iodine solution, in 100 parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant α-dimethylbenzylphenol polyoxyethylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts co-solvent potassium iodide, and the balance being water;
[0129] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0130] Comparative Example 3
[0131] A povidone-iodine solution, in 100 parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant α-methylbenzylphenol polyoxyethylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts co-solvent potassium iodide, and the balance being water;
[0132] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0133] Comparative Example 4
[0134] A povidone-iodine solution, in 100 parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dodecylphenol polyoxyethylene ether dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water;
[0135] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0136] Comparative Example 5
[0137] A povidone-iodine solution, in 100 parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts alkyl glycoside dispersant, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water;
[0138] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0139] Comparative Example 6
[0140] A povidone-iodine solution, in 100 parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.5 parts dispersant fatty alcohol polyoxyethylene ether, 0.2 parts stabilizer potassium iodate, 0.9 parts co-solvent potassium iodide, and the balance being water;
[0141] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0142] Comparative Example 7
[0143] A povidone-iodine solution, in 100 parts by weight: 20 parts polyvinylpyrrolidone, 10.5 parts iodine, 27 parts ethanol, 0.2 parts potassium iodate stabilizer, 0.9 parts potassium iodide co-solvent, and the balance being water;
[0144] In this embodiment, a concentrated solution of povidone-iodine was prepared according to method embodiment 4.
[0145] (I) Stability Testing
[0146] Samples: Povidone-iodine concentrate obtained in Examples 1-23 and povidone-iodine solution obtained in Comparative Examples 1-7.
[0147] Content detection (test) method: The content was detected according to the detection method of povidone-iodine solution in the "Veterinary Pharmacopoeia of the People's Republic of China (2020 Edition)".
[0148] Stability study: The product stability was assessed according to "GB / T 38499-2020 Method for Evaluation of Stability of Disinfectants". The data obtained are shown in Table 1:
[0149] Table 1. Sample content and pH value at 40℃
[0150]
[0151]
[0152] As can be seen from Table 1, Example 1 showed the best stability in iodine content and pH, while Comparative Examples 2-7 showed poor stability, with Comparative Example 7 showing the worst stability. This indicates that the addition of surfactants promoted the complexation of iodine and polyvinylpyrrolidone, thereby increasing the stability of the povidone-iodine concentrate.
[0153] The pH values of the povidone-iodine concentrates obtained in Examples 1-23 and the povidone-iodine solutions obtained in Comparative Examples 1-7 were adjusted to 2-2.5, and the samples were placed at 40°C for 20 days to observe their solubility. They were then diluted to a povidone-iodine content of 1%, and their surface tension was measured. The data are shown in Table 2.
[0154] Table 2. Solubility and surface tension of samples stored at 40℃ for 20 days.
[0155]
[0156]
[0157] As shown in Table 2, under low pH conditions, Examples 1-23 dissolved normally, and Comparative Example 1 dissolved normally as well. Comparative Examples 2, 3, and 6 dissolved slowly, and Comparative Example 7 was difficult to dissolve due to the absence of a surfactant. This indicates that the addition of a surfactant increased the solubility of the povidone-iodine concentrate.
[0158] (II) Iodine Complexation Test
[0159] The povidone-iodine concentrates obtained in Examples 1-23 and the povidone-iodine solutions obtained in Comparative Examples 1-7 were diluted to a povidone-iodine content of 5%. A 60-second free iodine identification test was performed at 25°C using the starch indicator filter paper method. The evaluation criteria were: filter paper color development time < 60s: poor; 65s ≥ 60s: acceptable; filter paper color development time > 65s: excellent. The results are shown in Table 3.
[0160] Table 3 Iodine complexation status
[0161]
[0162]
[0163] As shown in Table 3, the longer the filter paper takes to develop color, the less likely the iodine in the povidone-iodine solution is to become free and volatilize, indicating excellent iodine complexation and good stability of the povidone-iodine concentrate. In Example 1, the filter paper took the longest to develop color, indicating the best complexation and the best sample stability. Comparative Examples 1, 2, and 3 also showed relatively good iodine complexation. Comparative Example 7 showed the worst complexation.
[0164] (III) Salt Tolerance Test
[0165] Samples: Povidone-iodine concentrate obtained in Examples 1-23 and povidone-iodine solution obtained in Comparative Examples 1-7.
[0166] Prepare a 10% sea salt aqueous solution. Take 3g each of the povidone-iodine concentrate obtained in Examples 1-23 and the povidone-iodine concentrate obtained in Comparative Examples 1-7, add them to 100g of a 10% sea salt aqueous solution, stir, and observe the phenomenon.
[0167] Table 4 Salt Tolerance
[0168]
[0169]
[0170] As shown in Table 4, the povidone-iodine concentrates in Examples 1-23 still exhibited excellent solubility in high-concentration sea salt solutions, and Comparative Example 1 also showed normal solubility. Comparative Examples 2, 3, 4, 6, and 7 all showed abnormal solubility in high-salinity solutions, indicating salt intolerance.
[0171] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of the invention. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.
[0172] Finally, it should be noted that the embodiments disclosed in this invention are merely preferred embodiments of this invention and are only used to illustrate the technical solutions of this invention, not to limit it. Although this invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this invention.
Claims
1. A salt-resistant povidone-iodine concentrate, characterized in that: It includes the following components, in parts by weight of 100: 15-30 parts polyvinylpyrrolidone, 10-15 parts iodine, 25-35 parts solvent, 0.5-5 parts dispersant, 0-1 part stabilizer, 0.5-3 parts cosolvent, 0-5 parts pH adjuster, and the balance is water; The dispersant is dodecyl benzyl polyoxyethylene (9) ether; The stabilizer is potassium iodate; The co-solvent is potassium iodide.
2. The salt-resistant povidone-iodine concentrate according to claim 1, characterized in that: The solvent includes one or more of ethanol, ethylene glycol, n-propanol, isopropanol, propylene glycol, and glycerol.
3. The salt-resistant povidone-iodine concentrate according to claim 1, characterized in that: The pH adjuster includes one or more of sodium hydroxide, citric acid and sodium citrate, phosphoric acid and sodium dihydrogen phosphate.
4. A method for preparing a salt-resistant povidone-iodine concentrate according to any one of claims 1-3, characterized in that: Includes the following steps: (1) Dissolve polyvinylpyrrolidone in a solvent, then add iodine and co-solvent, stir and heat to 40-60℃ for complexation reaction for 2-5 hours; (2) After the reaction is complete, add a pH adjuster to adjust the pH of the solution to 3-6, then add a dispersant and a stabilizer, add water to 100 parts, and stir for 0.5-1h to obtain the solution.