Povidone iodine disinfectant as well as preparation method and application thereof

By coating povidone iodine with chitosan and combining quaternary ammonium surfactant and pH regulator, the problem of unstable effective iodine content and large changes in pH value of povidone iodine solution is solved, and high stability is achieved. Povidone iodine disinfectant, suitable for long-term use.

CN119318664APending Publication Date: 2025-01-17SHANGHAI YUKING WATER SOLUBLE MATERIAL TECH
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Patent Information

Application Number
CN202411434763.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-14
Publication Date
2025-01-17

AI Technical Summary

Technical Problem

The effective iodine content of existing povidone iodine solution is unstable and the pH value changes greatly, resulting in poor product quality and affecting clinical use.

Method used

Povidone iodine is coated with chitosan, and quaternary ammonium surfactant, potassium iodate, potassium iodide and pH regulator are added. The stable complex is formed by oxygen plasma modified chitosan and vacuum drying technology. Iodine is fixed and pH is adjusted.

Benefits of technology

It improves the stability and sustained release effect of effective iodine, maintains the stability of the pH value and effective iodine content for a long time, avoids solution stratification, and significantly improves the stability and convenience of use of disinfectants.

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Abstract

The invention belongs to the technical field of povidone iodine disinfectants, and discloses a povidone iodine disinfectant as well as a preparation method and application thereof. The raw materials comprise 3-6% of chitosan coated povidone iodine, 0.5-2% of a quaternary ammonium salt surfactant, 0.1-1% of potassium iodate, 0.1-0.5% of potassium iodide and the balance of water. The active component is chitosan-coated povidone iodine, firstly, chitosan is modified through oxygen plasma, the amino content of the chitosan is regulated and controlled, the number of oxygen-containing groups is increased, then povidone iodine is coated, and hydrogen bonds are formed between the modified chitosan and povidone iodine, so that a povidone iodine solid is fixed, and the stability of iodine is improved; the macromolecular structure of the chitosan can also play a role in slowly releasing free iodine. And meanwhile, the chitosan also has good biocompatibility and antibacterial activity, is small in irritation when being used for a specific part, and also can achieve an antibacterial effect.
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Description

Technical Field

[0001] The invention relates to the technical field of povidone-iodine disinfectants, and in particular to a povidone-iodine disinfectant and a preparation method and application thereof. Background Art

[0002] Povidone-iodine is a loose complex formed by combining elemental iodine and a polymer carrier. Povidone acts as a carrier and a solubilizer. It is a broad-spectrum, powerful bactericidal disinfectant that has a strong killing effect on viruses, bacteria, fungi and mold spores. Povidone-iodine aqueous solution does not have the disadvantages of iodine tincture, is light in color, easy to wash off, has little irritation to the mucous membrane, does not require ethanol deiodination, has no corrosive effect, and has low toxicity.

[0003] However, there are multiple iodine forms in povidone-iodine solution, in which there is a complex equilibrium relationship, and at different pH values, the effective iodine content varies greatly, and the povidone-iodine solution is very unstable in its pH value due to the dissociation and complexation of iodine, and the decline is large. The current commercially available povidone-iodine solution has an unstable effective iodine content, which has a serious impact on product quality, so medical institutions usually prepare it in clinical use, which brings multiple inconveniences. Prior art has a large number of studies on the improvement of the stability of povidone-iodine disinfectants, such as patent CN101310602A discloses a stable povidone-iodine disinfectant, which uses potassium iodate as a pH stabilizer, potassium iodide as a content stabilizer, and phosphate buffer as a solution pH stabilizer, and also contains more glycerol, but the povidone-iodine disinfectant of the formula is placed for a long time and is easy to be layered. For example, patent CN106798749A discloses a povidone-iodine film-forming disinfectant, which is composed of 5% povidone-iodine, 0.1-0.5% carbomer, 1-10% PVP and 0.1-0.5% potassium iodate. The pH of the solution is stable and the problem of stratification of the disinfectant solution is solved. However, the pH value and effective iodine content of the disinfectant solution decrease significantly after being placed for 6 months.

[0004] Therefore, how to provide a povidone-iodine disinfectant with a stable effective iodine content, small change in solution pH value, and long-term stability is a problem that urgently needs to be solved. Summary of the invention

[0005] The purpose of the present invention is to provide a povidone-iodine disinfectant and a preparation method and application thereof, so as to solve the problems of unstable effective iodine content and large change in pH value of the povidone-iodine solution in the prior art.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The present invention provides a povidone-iodine disinfectant, comprising the following raw materials in percentage by weight:

[0008] Chitosan coated with povidone iodine 3-6%, quaternary ammonium salt surfactant 0.5-2%, potassium iodate 0.1-1%, potassium iodide 0.1-0.5%, and the balance is water;

[0009] Wherein, the preparation method of chitosan-coated povidone-iodine comprises the following steps:

[0010] Chitosan is modified by oxygen plasma, mixed with povidone iodine and water, reacted under a protective atmosphere, and finally vacuum dried to obtain the chitosan-coated povidone iodine.

[0011] Preferably, in the above-mentioned povidone-iodine disinfectant, the povidone-iodine disinfectant further comprises a pH regulator; the pH regulator adjusts the pH of the povidone-iodine disinfectant to 5-6.

[0012] Preferably, in the above-mentioned povidone-iodine disinfectant, the pH regulator is sodium hydroxide.

[0013] Preferably, in the above-mentioned povidone-iodine disinfectant, the parameters of the oxygen plasma modification are: power of 100-500W; time of 5-25min; vacuum degree of 20-100Pa.

[0014] Preferably, in the above-mentioned povidone-iodine disinfectant, the mass ratio of chitosan to povidone-iodine is 1-5:1-7.

[0015] Preferably, in the above-mentioned povidone-iodine disinfectant, the temperature of vacuum drying is 40-60° C.; the time of vacuum drying is 6-14 h; and the vacuum degree of vacuum drying is 10 Pa.

[0016] Preferably, in the above-mentioned povidone-iodine disinfectant, the reaction time under the protective atmosphere is 1 to 3 hours.

[0017] Preferably, in the above-mentioned povidone-iodine disinfectant, the quaternary ammonium salt surfactant is benzalkonium chloride or benzalkonium bromide.

[0018] The present invention also provides a method for preparing a povidone-iodine disinfectant, comprising the following steps:

[0019] Potassium iodide, quaternary ammonium salt surfactant and water are mixed, and then chitosan-coated povidone iodine and potassium iodate are added in sequence, and finally a pH regulator is used to adjust the pH to 5-6 to obtain a povidone iodine disinfectant.

[0020] The invention also provides an application of a povidone-iodine disinfectant in skin disinfection.

[0021] It can be seen from the above technical solution that compared with the prior art, the present invention has the following beneficial effects:

[0022] The active component of the invention is chitosan coated povidone iodine. First, chitosan is modified by oxygen plasma to adjust the amino content and increase the number of oxygen-containing groups. Then, povidone iodine is coated to form hydrogen bonds between the modified chitosan and povidone iodine, thereby fixing the povidone iodine solid and improving the stability of iodine. The macromolecular structure of chitosan can also play a role in slow release of free iodine. At the same time, chitosan also has good biocompatibility and antibacterial properties. It is less irritating when used in specific parts and can also achieve antibacterial effects.

[0023] The povidone-iodine disinfectant of the present invention utilizes coated povidone-iodine and is supplemented with a quaternary ammonium salt surfactant, a stabilizer, and a pH regulator, thereby further improving the sustained-release effect of free iodine and the stability of the solution, maintaining a stable effective iodine content, and achieving a good antibacterial and disinfection effect. DETAILED DESCRIPTION

[0024] The present invention provides a povidone-iodine disinfectant, comprising the following raw materials in percentage by weight:

[0025] The chitosan is coated with 3-6% povidone iodine, 0.5-2% quaternary ammonium salt surfactant, 0.1-1% potassium iodate, 0.1-0.5% potassium iodide, and the balance is water.

[0026] In the present invention, the mass percentage of the chitosan-coated povidone-iodine is preferably 3.2-5.7%, more preferably 3.5-4.5%, and more preferably 4%.

[0027] In the present invention, the mass percentage of the quaternary ammonium salt surfactant is preferably 0.7-1.7%, more preferably 0.9-1.5%, and even more preferably 1%.

[0028] In the present invention, the mass percentage of the potassium iodate is preferably 0.2-0.8%, more preferably 0.3-0.7%, and more preferably 0.6%.

[0029] In the present invention, the mass percentage of the potassium iodide is preferably 0.1-0.4%, more preferably 0.1-0.2%, and more preferably 0.1%.

[0030] In the present invention, the povidone-iodine disinfectant further comprises a pH adjuster; the pH of the povidone-iodine disinfectant adjusted by the pH adjuster is preferably 5 to 6, more preferably 5.2 to 5.8, and more preferably 5.62.

[0031] In the present invention, the pH adjuster is preferably sodium hydroxide.

[0032] In the present invention, the quaternary ammonium salt surfactant is preferably benzalkonium chloride or benzalkonium bromide, and more preferably benzalkonium chloride.

[0033] In the present invention, the preparation method of chitosan-coated povidone-iodine comprises the following steps:

[0034] Chitosan is modified by oxygen plasma, mixed with povidone iodine and water, reacted under a protective atmosphere, and finally vacuum dried to obtain the chitosan-coated povidone iodine.

[0035] In the present invention, the parameters of the oxygen plasma modification are: the power is preferably 100-500W, more preferably 150-400W, more preferably 250W; the time is preferably 5-25min, more preferably 8-20min, more preferably 15min; the vacuum degree is preferably 20-100Pa, more preferably 50-80Pa, more preferably 60Pa.

[0036] In the present invention, the mass ratio of chitosan to povidone-iodine is preferably 1-5:1-7, more preferably 2-4:3-6, and even more preferably 4:5.

[0037] In the present invention, the mass ratio of chitosan to water is preferably 1-5:20-100, more preferably 2-4:40-70, and even more preferably 4:50.

[0038] In the present invention, the protective atmosphere is preferably nitrogen.

[0039] In the present invention, the reaction time under the protective atmosphere is preferably 1 to 3 hours, more preferably 2 to 3 hours, and more preferably 3 hours.

[0040] In the present invention, the reaction process under a protective atmosphere also includes stirring; the stirring speed is preferably 500 to 1000 rpm, more preferably 600 to 900 rpm, and more preferably 800 rpm.

[0041] In the present invention, the vacuum drying temperature is preferably 40-60°C, more preferably 45-60°C, and more preferably 60°C; the vacuum drying time is preferably 6-14h, more preferably 8-12h, and more preferably 10h; the vacuum degree of the vacuum drying is preferably 10Pa.

[0042] The present invention also provides a method for preparing a povidone-iodine disinfectant, comprising the following steps:

[0043] Potassium iodide, quaternary ammonium salt surfactant and water are mixed, and then chitosan-coated povidone iodine and potassium iodate are added in sequence, and finally a pH regulator is used to adjust the pH to 5-6 to obtain a povidone iodine disinfectant.

[0044] The invention also provides an application of a povidone-iodine disinfectant in skin disinfection.

[0045] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0046] Example 1

[0047] This embodiment provides a povidone-iodine disinfectant, comprising the following raw materials in percentage by weight:

[0048] Chitosan is coated with 5% povidone iodine, 1% benzalkonium chloride, 0.3% potassium iodate, 0.2% potassium iodide, and a pH regulator, sodium hydroxide, to adjust the pH to 5.62, and the balance is water.

[0049] The preparation method of the above-mentioned povidone iodine disinfectant comprises the following steps:

[0050] (1) Chitosan was modified by oxygen plasma at a power of 350 W and a vacuum degree of 80 Pa for 18 min, then mixed evenly with povidone iodine and water at a mass ratio of 2:3:40, stirred and reacted at 600 rpm for 2 h in a nitrogen atmosphere, and finally vacuum dried at a vacuum degree of 10 Pa and 60° C. for 12 h to obtain chitosan coated with povidone iodine;

[0051] (2) Potassium iodide, benzalkonium chloride and water are stirred and mixed evenly, then chitosan-coated povidone iodine is added and stirred and mixed evenly, potassium iodate is added and stirred and mixed evenly, and finally sodium hydroxide is used to adjust the pH to 5.62 to obtain a povidone iodine disinfectant.

[0052] Example 2

[0053] This embodiment provides a povidone-iodine disinfectant, comprising the following raw materials in percentage by weight:

[0054] Chitosan is coated with 4% povidone iodine, 0.7% benzalkonium bromide, 0.5% potassium iodate, 0.1% potassium iodide, and a pH regulator, sodium hydroxide, to adjust the pH to 5.45, and the balance is water.

[0055] The preparation method of the above-mentioned povidone iodine disinfectant comprises the following steps:

[0056] (1) Chitosan was modified by oxygen plasma at a power of 200 W and a vacuum degree of 50 Pa for 10 min, then mixed with povidone iodine and water at a mass ratio of 4:4:30, stirred and reacted at 1000 rpm in a nitrogen atmosphere for 1 h, and finally vacuum dried at a vacuum degree of 10 Pa and 60° C. for 8 h to obtain chitosan coated with povidone iodine;

[0057] (2) Potassium iodide, benzalkonium bromide and water are stirred and mixed evenly, then chitosan-coated povidone iodine is added and stirred and mixed evenly, potassium iodate is added and stirred and mixed evenly, and finally sodium hydroxide is used to adjust the pH to 5.45 to obtain a povidone iodine disinfectant.

[0058] Example 3

[0059] This embodiment provides a povidone-iodine disinfectant, comprising the following raw materials in percentage by weight:

[0060] Chitosan is coated with 4.5% povidone iodine, 1.5% benzalkonium bromide, 0.6% potassium iodate, 0.5% potassium iodide, and a pH regulator, sodium hydroxide, to adjust the pH to 5.27, and the balance is water.

[0061] The preparation method of the above-mentioned povidone iodine disinfectant comprises the following steps:

[0062] (1) Chitosan was modified by oxygen plasma at a power of 250 W and a vacuum degree of 80 Pa for 12 min, then mixed evenly with povidone iodine and water at a mass ratio of 4:5:50, stirred and reacted at 600 rpm for 3 h in a nitrogen atmosphere, and finally vacuum dried at a vacuum degree of 10 Pa and 60° C. for 10 h to obtain chitosan coated with povidone iodine;

[0063] (2) Potassium iodide, benzalkonium bromide and water are stirred and mixed evenly, then chitosan-coated povidone iodine is added and stirred and mixed evenly, potassium iodate is added and stirred and mixed evenly, and finally sodium hydroxide is used to adjust the pH to 5.27 to obtain a povidone iodine disinfectant.

[0064] Example 4

[0065] This embodiment provides a povidone-iodine disinfectant, comprising the following raw materials in percentage by weight:

[0066] Chitosan is coated with 6% povidone iodine, 1% benzalkonium chloride, 0.2% potassium iodate, 0.5% potassium iodide, and a pH regulator, sodium hydroxide, to adjust the pH to 5.86, and the balance is water.

[0067] The preparation method of the above-mentioned povidone iodine disinfectant comprises the following steps:

[0068] (1) Chitosan was modified by oxygen plasma at a power of 500 W and a vacuum degree of 50 Pa for 5 min, then mixed evenly with povidone iodine and water at a mass ratio of 1:5:80, stirred and reacted at 1000 rpm for 2 h in a nitrogen atmosphere, and finally vacuum dried at a vacuum degree of 10 Pa and 40° C. for 14 h to obtain chitosan coated with povidone iodine;

[0069] (2) Potassium iodide, benzalkonium chloride and water are stirred and mixed evenly, then chitosan-coated povidone iodine is added and stirred and mixed evenly, potassium iodate is added and stirred and mixed evenly, and finally sodium hydroxide is used to adjust the pH to 5.86 to obtain a povidone iodine disinfectant.

[0070] Comparative Example 1

[0071] This comparative example provides a povidone-iodine disinfectant, which is specifically referred to Example 1, except that chitosan is not modified by oxygen plasma.

[0072] Comparative Example 2

[0073] This comparative example provides a povidone-iodine disinfectant, which is specifically referred to Example 1, except that the chitosan-coated povidone-iodine is replaced with chitosan 2% and povidone-iodine 3%.

[0074] Comparative Example 3

[0075] This comparative example provides a povidone-iodine disinfectant, which is specifically referred to in Example 1, except that the chitosan-coated povidone-iodine is replaced with povidone-iodine.

[0076] Comparative Example 4

[0077] This comparative example provides a povidone-iodine disinfectant, which is specifically referred to in Example 1, except that it does not contain benzalkonium chloride.

[0078] The pH value and the available iodine content of the povidone-iodine disinfectants of Examples 1 to 4 and Comparative Examples 1 to 4 were measured immediately after preparation (the available iodine content was measured by 1 mol / L sodium thiosulfate titration method), recorded as 0 month, and then placed for 1 month, 2 months, 3 months, and 5 months (placement conditions were 25°C ± 2°C, relative humidity 75% ± 5%), respectively, and the pH value and the available iodine content were measured. The test results are shown in Table 1.

[0079] Table 1 pH value and effective iodine content of povidone iodine disinfectant

[0080]

[0081]

[0082] As shown in Table 1, the pH value and the effective iodine content of the povidone-iodine disinfectant prepared by the present invention change slightly during long-term storage, and there is no stratification, and the solution has high stability. The effective iodine content can reach the concentration at the time of initial preparation after being placed for 1 to 3 months, indicating that the formula of the present invention can achieve the effect of slow release of effective iodine and weaken the influence of pH value changes on the effective iodine content.

[0083] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A povidone-iodine disinfectant, characterized in that: Contains the following raw materials in percentage by weight: Chitosan coated with povidone iodine 3-6%, quaternary ammonium salt surfactant 0.5-2%, potassium iodate 0.1-1%, potassium iodide 0.1-0.5%, and the balance is water; Wherein, the preparation method of chitosan-coated povidone-iodine comprises the following steps: Chitosan is modified by oxygen plasma, mixed with povidone iodine and water, reacted under a protective atmosphere, and finally vacuum dried to obtain the chitosan-coated povidone iodine.

2. A povidone-iodine disinfectant according to claim 1, characterized in that, The povidone-iodine disinfectant further comprises a pH regulator; the pH regulator regulates the pH of the povidone-iodine disinfectant to 5-6.

3. A povidone-iodine disinfectant according to claim 2, characterized in that, The pH regulator is sodium hydroxide.

4. A povidone-iodine disinfectant according to claim 3, characterized in that, The parameters of the oxygen plasma modification are: power of 100-500W; time of 5-25min; vacuum degree of 20-100Pa.

5. A povidone-iodine disinfectant according to claim 1 or 4, characterized in that, The mass ratio of chitosan to povidone iodine is 1-5:1-7.

6. A povidone-iodine disinfectant according to claim 5, characterized in that, The temperature of the vacuum drying is 40-60° C.; the time of the vacuum drying is 6-14 hours; and the vacuum degree of the vacuum drying is 10 Pa.

7. A povidone-iodine disinfectant according to claim 6, characterized in that, The reaction time under the protective atmosphere is 1 to 3 hours.

8. A povidone-iodine disinfectant according to claim 5, characterized in that: The quaternary ammonium salt surfactant is benzalkonium chloride or benzalkonium bromide.

9. The method for preparing a povidone-iodine disinfectant according to any one of claims 1 to 8, characterized in that: The following steps are involved: Potassium iodide, quaternary ammonium salt surfactant and water are mixed, and then chitosan-coated povidone iodine and potassium iodate are added in sequence, and finally a pH regulator is used to adjust the pH to 5-6 to obtain a povidone iodine disinfectant.

10. Use of a povidone-iodine disinfectant according to any one of claims 1 to 8 in skin disinfection.

Citation Information

Patent Citations

  • Stable type povidone iodine disinfectant and preparation method thereof

    CN101310602A

  • Povidone-iodine film-forming disinfectant, preparation method and application thereof

    CN106798749A