CN113288913A - Povidone iodine solution and preparation method thereof - Google Patents

Povidone iodine solution and preparation method thereof Download PDF

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CN113288913A
CN113288913A CN202110571717.1A CN202110571717A CN113288913A CN 113288913 A CN113288913 A CN 113288913A CN 202110571717 A CN202110571717 A CN 202110571717A CN 113288913 A CN113288913 A CN 113288913A
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povidone
iodine
iodine solution
solution
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庄若飞
庄若明
骆桂红
李惠静
董星
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Xiamen Huiying Animal Pharmaceutical Co ltd
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Xiamen Huiying Animal Pharmaceutical Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

The invention discloses a povidone iodine solution which is prepared from the following components in parts by weight: 30-50 parts of povidone iodine, 30-40 parts of ethanol, 3-30 parts of water, 2-5 parts of potassium iodide, 2-4 parts of a stabilizer and 1.4-2.4 parts of a pH regulator. The preparation method comprises the steps of dissolving, mixing and the like in equipment with the polytetrafluoroethylene coating. The invention has scientific and reasonable formula composition and unique process, is viscous liquid with the effective iodine content of 3-5 percent, is diluted into solution with the effective iodine content of 0.5-1 percent by adding water, has self-thickening effect and strong stability, is not influenced by various factors such as water hardness, pH value and the like when in use, has good dispersibility, lasting effect and thorough sterilization; the adhesive has better adhesiveness, and the disinfection efficiency is improved; no irritation to skin, mucous membrane and eyes; can kill pathogens such as bacteria, spores, viruses and the like in a short time and at a low concentration; meanwhile, the feed additive has the effects of lasting moisture preservation and chapping prevention, and is widely applied to different breeding varieties.

Description

Povidone iodine solution and preparation method thereof
Technical Field
The invention relates to the technical field of veterinary antibacterial disinfectant preparations, in particular to a preparation method and application of povidone iodine solution.
Background
The povidone iodine is a complex of polyvinylpyrrolidone-K30 (PVP-K30) and iodine, takes active iodine as a main sterilization component, and has strong killing effect on common bacteria such as staphylococcus aureus, pseudomonas aeruginosa, escherichia coli, candida albicans, hepatitis B virus, trichomonas vaginalis, spores and the like. It has the advantages of low volatility, good water solubility, mild and lasting action and safe use, and is a novel high-efficiency, broad-spectrum and low-toxicity disinfectant for external use.
In the existing technology for preparing povidone iodine solution, if the content of prepared effective iodine is high, the film forming property, the stability and the sterilization effect are poor, the viscosity after dilution is greatly reduced, the adhesive force, the stability and the sterilization effect are also worse along with the dilution, and if the povidone iodine solution achieves better stability and adhesiveness, a complex and tedious process is often needed. Patent application No. CN201610265563.2 provides a preparation method of povidone iodine concentrated solution, but the preparation process is complex, the energy consumption is large, the requirement on equipment is high, the required raw and auxiliary materials are complex, and the production time is long. Therefore, the development of the povidone iodine solution which has good adhesiveness, is quickly dissolved during dilution, has high effective iodine content, has excellent adhesiveness, stability and bactericidal power of stock solution and diluent, and has unique process and low equipment requirement has very important significance.
Disclosure of Invention
Based on the above, the invention provides the povidone iodine solution and the preparation method thereof, the formula composition is scientific and reasonable, the process is unique, the povidone iodine solution is viscous liquid with the effective iodine content of 3% -5%, the povidone iodine solution is diluted by adding water into the liquid to form a solution with the effective iodine content of 0.5% -1%, the povidone iodine solution also has a self-thickening effect and strong stability, is not influenced by various factors such as water hardness, pH value and the like during use, and has good dispersibility, lasting effect and thorough sterilization; the adhesive has better adhesiveness, and the disinfection efficiency is improved; no irritation to skin, mucous membrane and eyes; can kill pathogens such as bacteria, spores, viruses and the like in a short time and at a low concentration; meanwhile, the feed additive has the effects of lasting moisture preservation and chapping prevention, and is widely applied to different breeding varieties.
The invention is realized by the following technical scheme:
the povidone-iodine solution is prepared from the following components in parts by weight: 30-50 parts of povidone iodine, 30-40 parts of ethanol, 3-30 parts of water, 2-5 parts of potassium iodide, 2-4 parts of a stabilizer and 1.4-2.4 parts of a pH regulator.
The stabilizer is hydroxypropyl methyl cellulose, and the viscosity is more than 100mPa & s.
The pH regulator is sodium tripolyphosphate with a sodium tripolyphosphate content of 85.0 wt% or more, and total phosphate (P as P)2O5Calculated) 56.0 wt% to 58.0 wt%.
A preparation method of povidone iodine solution comprises the following components in parts by weight: 30-50 parts of povidone iodine, 30-40 parts of ethanol, 3-30 parts of water, 2-5 parts of potassium iodide, 2-4 parts of hydroxypropyl methyl cellulose and 1.4-2.4 parts of sodium tripolyphosphate; the preparation steps are as follows:
the method comprises the following steps: weighing potassium iodide and water according to the prescription amount, dissolving, and filling into a specific solution preparation container to form a body system 1;
step two: adding povidone iodine and ethanol with the prescribed amount into the system 1, placing an impeller of a dispersion machine at the center of a container, lowering the impeller to the lowest position, starting the machine to adjust the rotating speed to 1200r/min, and stirring for 30 minutes to form a system 2;
step three: adding hydroxypropyl methyl cellulose and sodium tripolyphosphate into the system 2, and stirring for 30 minutes to obtain the povidone-iodine solution.
The special preparation container and the dispersion machine are made of metal materials, and the surfaces of the special preparation container and the dispersion machine are provided with polytetrafluoroethylene coatings.
The special preparation container is provided with an inner barrel and an outer barrel which are sleeved together, a cooling liquid chamber is formed between the inner barrel and the outer barrel, and the cooling liquid chamber is provided with a cooling liquid inlet and a cooling liquid outlet.
After the scheme is adopted, the invention has the beneficial effects that:
firstly, the adopted preparation process only needs dissolution and mixing, and has simple process, simple and convenient operation, short production time and less energy consumption;
secondly, the dissolving and mixing container and the dispersing machine are made of metal materials of polytetrafluoroethylene coatings, have the characteristics of acid resistance, alkali resistance and various organic solvents resistance, are almost insoluble in all solvents, and meanwhile, the polytetrafluoroethylene coatings have the characteristics of high temperature resistance and extremely low friction coefficient, are suitable for the production of povidone iodine solution, and enable the dispersion to be more homogeneous;
the container is provided with a cooling system, and the cooling liquid can absorb heat generated by stirring in the mixing process, so that the temperature of the raw materials is reduced, and the stability of the product quality is further ensured;
fourthly, the added hydroxypropyl methyl cellulose has the functions of thickening, stabilizing solution and keeping moisture, and the hydroxypropyl methyl cellulose still has the function of self-thickening after being diluted into different concentrations after being prepared into the solution;
fifthly, the added sodium tripolyphosphate not only has the functions of adjusting pH and thickening, but also is matched with hydroxypropyl methyl cellulose, so that the product has good adhesiveness, the maintenance time of the disinfection effect of the povidone iodine solution is prolonged, the disinfection efficiency is improved, and the dissolution effect of the povidone iodine is also improved together with potassium iodide;
sixthly, the prepared povidone iodine solution is a liquid with the effective iodine content of 3% -5%, and is diluted by adding water to prepare a 0.5% -1% solution, so that the povidone iodine solution is widely applied to different breeding varieties.
(1) When the bactericidal composition is used for aquaculture, the dissolution speed in water is high, diseases such as hemorrhage, gill rot, furuncle, skin rot and the like caused by bacteria such as vibrio aeromonas hydrophila, edwardsiella and the like can be prevented and controlled, the dispersion is uniform from top to bottom, the dispersibility is good, the effect is durable, the sterilization is more thorough, the water quality can be prevented and controlled at the bottom, and a healthy culture environment is created;
(2) when used for livestock and poultry, the disinfectant can be used for spraying and disinfecting animals, breeding houses and drinking water lines, can inhibit harmful bacteria, prevent and control digestive tract infection, diarrhea and dysentery, and reduce the possibility of virus oral infection;
(3) the infection after the shearing of the teeth of the piglets, the wound treatment after the castration of the piglets, the knee abrasion of the piglets on the obstetric table in 3-5 days old, the wound surface and the sow hoof fissure caused by the support-taking and the biting of the pigs, such as pigsty folding and hurdling, can be prevented, the wound healing is fast, and the irritation to the wound is avoided;
(4) can be used for scrubbing the antenatal and postnatal breasts, the hip, the abdomen and the pudendum of the sow, and can prevent mastitis, metritis and the like;
(5) can be used for medicated bath before and after milking of cow breast, and can prevent metritis and mastitis of cow, and has the advantages of mild condition, no irritation, good skin affinity, low dosage, and good and bright and elastic cow nipple after long-term use.
(6) The ointment can be applied to the affected part to improve dermatitis, rash and tinea, promote wound healing, dissipate induration, and has the effects of keeping moisture and preventing chapping.
Drawings
FIGS. 1 to 3 are graphs showing the results of pH stability after 10-fold dilution of povidone-iodine solutions and comparative examples according to the present invention;
FIG. 4 is a graph of the bacteriostatic results of 4000-fold dilutions of 1% available iodine povidone-iodine solution;
FIG. 5 is a graph showing the dissolution and dispersion of povidone-iodine solution of the present invention in water;
FIG. 6 is a graph showing the condition of the breasts of the cows after the mastitis is cured in the control group and the test group.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein.
Comparative examples 1 to 18 and examples 1 to 6: the component formulations are shown in tables 1-3.
TABLE 1
Figure BDA0003082818290000051
TABLE 2
Figure BDA0003082818290000061
TABLE 3
Figure BDA0003082818290000062
Figure BDA0003082818290000071
TABLE 4
Figure BDA0003082818290000072
Figure BDA0003082818290000081
Comparative examples 1 to 6 preparation process:
1) sequentially adding PVP-K30, iodine and potassium iodide (dissolved by a small amount of water in advance) in a formula amount into a reaction kettle containing ethanol, continuously stirring in the adding process, controlling the reaction temperature to be 40-60 ℃, stirring until the iodine and the potassium iodide are completely dissolved, and fully reacting for 3-5 hours to obtain an ethanol solution of iodine-PVP-K30, which is marked as solution A;
2) adding the thickening agent into water, fully stirring until the thickening agent is completely dissolved, and recording the obtained water solution as liquid B;
3) weighing the humectant and the emulsifier according to the formula ratio, and fully stirring until the humectant and the emulsifier are completely dissolved to obtain an organic solution which is marked as solution C;
4) transferring the solution A into a high-speed shearing emulsifying machine, sequentially adding the solution B, the solution C, a dispersing agent and a synergist under continuous stirring, fully emulsifying for 5-8 h, preparing a conditioner into a solution, and adjusting the pH value of the povidone iodine concentrated solution to 3.0-6.5;
5) and (3) after standing and cooling, detecting the effective iodine content and the pH value of the povidone iodine concentrated solution, and discharging, filling, packaging and warehousing after the povidone iodine concentrated solution is qualified.
Comparative examples 7 to 21, examples 1 to 6 preparation processes:
the method comprises the following steps: weighing potassium iodide and water according to the prescription amount, dissolving, and then filling into a specific container to form a body system 1;
step two: adding povidone iodine and ethanol with the prescribed amount into the system 1, placing an impeller of a dispersion machine at the center of a container, lowering the impeller to the lowest position, starting the machine to adjust the rotating speed to 1200r/min, and stirring for 30 minutes to form a system 2;
step three: and adding a stabilizing agent and a pH regulator into the system 2, and stirring for 30 minutes to obtain the povidone-iodine solution.
Test one: the invention relates to comparison and analysis of preparation process of povidone iodine solution
Note: "/" indicates no specific setting or requirement
TABLE 5
Figure BDA0003082818290000091
And (2) test II: the invention relates to an appearance stability test of povidone iodine solution
Povidone iodine solution for testing: the preparation was carried out by the methods of comparative examples 1 to 21 and examples 1 to 6.
And observing the appearance stability of the povidone-iodine solution in 0 month, 1 month, 3 months, 6 months, 12 months and 24 months under the conditions of normal temperature and light protection.
The test results are shown in table 6:
note: "/" indicates no testing was performed.
TABLE 6
Figure BDA0003082818290000101
Figure BDA0003082818290000111
Figure BDA0003082818290000121
As can be seen from Table 6, in comparative example 1 and comparative example 2, the solution was precipitated and could not be completely dissolved due to the addition of less potassium iodide; comparative example 9 had already slightly stratified at month 1; comparative example 10 had slight delamination at month 6; comparative examples 14, 15 began to stratify at month 1; comparative examples 18 and 20 gas was generated when sodium bicarbonate and anhydrous sodium carbonate were added; from the above comparative examples and examples, it can be seen that sodium carboxymethylcellulose and hydroxyethylcellulose are not suitable as thickeners, and sodium hydroxide, potassium hydroxide, sodium carbonate and sodium bicarbonate are not suitable as pH adjusters.
And (3) test III: the invention relates to a pH stability test after 10-fold dilution of a povidone-iodine solution
Povidone iodine solution for testing: prepared by the methods of comparative examples 3-6, 14-17, 19 and 21 and examples 1-6.
The test method comprises the following steps: the pH was determined by 10-fold dilution at 25 deg.C
And (3) testing time: the measurement is carried out for 0 month, 1 month, 3 months, 6 months, 12 months and 24 months respectively.
The test results are shown in Table 7 and attached figures 1-3:
TABLE 7
Figure BDA0003082818290000131
Figure BDA0003082818290000141
From Table 7 and FIGS. 1 to 3, it can be seen that the pH regulators used in comparative examples 14 to 16 were sodium hydroxide, potassium hydroxide had a relatively rapid pH drop over a period of time, and the buffering effect was not as good as that of the other regulators, and that comparative examples 3 to 6 had a relatively gentle pH drop over a period of time, but the buffering effect was not as good as that of examples 1 to 6.
And (4) testing: the invention relates to a povidone iodine solution and the viscosity of the solution after being diluted by 10 times
Povidone iodine solution for testing: prepared by the method of comparative examples 3-13 and examples 1-6.
The test conditions are as follows: detecting the viscosity of the stock solution and the 10 times of the diluent at 25 DEG C
The test results are shown in table 8:
TABLE 8
Viscosity (25 ℃, mpa.s) Stock solution 10 times of diluent
Comparative example 3 1650 1350
Comparative example 4 5120 1840
Comparative example 5 8740 6210
Comparative example 6 1340 1280
Comparative example 7 1210 1160
Comparative example 8 3440 2100
Comparative example 9 1360 1150
Comparative example 10 6540 5220
Comparative example 11 3470 2280
Comparative example 12 3650 2130
Comparative example 13 4830 3670
Example 1 11070 10080
Example 2 12110 11890
Example 3 10360 9990
Example 4 10050 9970
Example 5 9880 9620
Example 6 10080 9940
From the above table, it is known that the viscosities of comparative examples 3 to 13 are all low, the viscosity reduction range after the solution dilution is large, the hydroxypropyl methylcellulose adopted in examples 1 to 6 has a self-thickening effect, and the solution after dilution still has good adhesiveness.
And (5) testing: the invention relates to a povidone iodine solution and the condition of the stability of the effective iodine content after the povidone iodine solution is diluted by 10 times
Povidone iodine solution for testing: the preparation method is adopted for preparing the materials by the methods of comparative examples 1-6 and examples 1-6.
(1) Effective iodine test conditions: the detection is carried out according to the related requirements of povidone iodine solution in the pharmacopoeia of the people's republic of China 2015 edition, and the specific method is as follows: about 1g of the product was weighed out precisely, placed in a beaker, added with 120ml of water, stirred to dissolve, and titrated with sodium thiosulfate titrant (0.1mol/L) by potentiometric titration. Each 1ml of sodium thiosulfate titrant (0.1mol/L) corresponds to 12.69mg of I.
(2) And (3) testing time: 0. measurements were performed for 1, 3, 6, 9, 12, 18, and 24 months, respectively.
The test results are shown in tables 9-10:
TABLE 9 Povidone iodine solution effective iodine stability
Available iodine (%) 0 month 1 month 3 months old 6 months old 9 months old 12 months old 18 months old 24 months
Example 1 2.96 2.95 2.94 2.93 2.91 2.89 2.79 2.78
Example 2 3.47 3.46 3.44 3.34 3.32 3.28 3.27 3.26
Example 3 3.98 3.96 3.92 3.89 3.84 3.77 3.76 3.75
Example 4 4.47 4.47 4.46 4.39 4.32 4.26 4.23 4.22
Example 5 4.76 4.76 4.74 4.71 4.62 4.55 4.50 4.48
Example 6 4.98 4.97 4.96 4.91 4.83 4.77 4.74 4.73
TABLE 10 stability of available iodine after 10-fold dilution of povidone-iodine solution
Available iodine (%) 0 month 1 month 3 months old 6 months old 9 months old 12 months old 18 months old 24 months
Example 1 0.29 0.29 0.29 0.28 0.28 0.27 0.26 0.26
Example 2 0.34 0.34 0.34 0.33 0.33 0.32 0.32 0.31
Example 3 0.39 0.39 0.39 0.38 0.38 0.37 0.37 0.36
Example 4 0.44 0.44 0.44 0.43 0.43 0.42 0.42 0.41
Example 5 0.47 0.47 0.47 0.46 0.46 0.45 0.45 0.44
Example 6 0.49 0.49 0.49 0.49 0.48 0.47 0.46 0.46
And (6) test six: the invention relates to a povidone iodine solution and a stability test of effective iodine content for an accelerated test after dilution by 10 times
Povidone iodine solution for testing: examples 1-6.
An appropriate packaging container (a bottle made of PE material is adopted in the test), a stability acceleration test is carried out under the conditions of the temperature of 40 +/-2 ℃ and the humidity of 75 +/-5%, and the stability condition of the povidone-iodine solution and the povidone-iodine solution diluted by 10 times within six months is determined.
The test results are shown in tables 11-12:
TABLE 11 stability of available iodine content of Povidone iodine solution
Available iodine (%) 0 month 1 month 3 months old 6 months old
Example 1 2.96 2.92 2.86 2.78
Example 2 3.47 3.42 3.32 3.26
Practice ofExample 3 3.98 3.94 3.85 3.74
Example 4 4.47 4.42 4.30 4.21
Example 5 4.76 4.70 4.57 4.48
Example 6 4.98 4.94 4.81 4.72
TABLE 12 stability of available iodine content after 10-fold dilution of povidone-iodine solution
Available iodine (%) 0 month 1 month 3 months old 6 months old
Example 1 0.29 0.28 0.28 0.27
Example 2 0.34 0.34 0.33 0.32
Example 3 0.39 0.38 0.37 0.37
Example 4 0.44 0.43 0.43 0.42
Example 5 0.47 0.47 0.46 0.45
Example 6 0.49 0.49 0.48 0.47
Test seven: the invention relates to a bacteriostatic effect of povidone iodine solution
Povidone iodine solution for test preparation according to the method of example 6, the povidone iodine solution of the present invention is diluted with water to a solution with an effective iodine content of 1.0%.
The test steps are as follows:
firstly, transferring 4.5ml of neutralizing agent into a small test tube by using a liquid transfer gun in an ultraclean workbench for 21 tubes. Diluting povidone iodine solution with effective iodine content of 1% by 250 times, 500 times, 1000 times, 2000 times, 4000 times and 8000 times, and counting 6 dilutions, wherein 5ml of each small test tube is removed in each dilution, and 3 small test tubes are removed in each dilution;
second, the bacteria concentration in the clean bench is 10 by using a liquid-transferring gun8Respectively adding 50 μ l of cfu/ml of escherichia coli, staphylococcus aureus and salmonella into 5ml of 6 dilutions, mixing uniformly, transferring 0.5ml of sample into 4.5ml of neutralizing agent after reacting for 30s, and neutralizing for 10min to obtain a test sample;
thirdly, transferring 5ml of physiological saline into small test tubes by a liquid transfer gun in the ultra-clean workbench for three times, dividing into 3 small test tubes in total, and transferring the bacteria concentration to 10 by the liquid transfer gun8Respectively adding 50 μ l of cfu/ml Escherichia coli, Staphylococcus aureus and Salmonella into 5ml physiological saline, mixing, transferring 0.5ml to 4.5ml neutralizer, and neutralizing for 10min to obtain blank reference substance;
fourthly, uniformly mixing the test samples, respectively transferring 50 mu l of the test samples to a culture medium on a culture plate by using a liquid transfer gun, and uniformly coating the test samples to be used as a test group; mixing blank reference substances, transferring 50 μ l of the reference substances to culture medium on a culture plate with a pipette, and uniformly coating to obtain a control group; the cells were cultured in an inverted state in a 36 ℃ incubator for 24 hours.
The test results are shown in table 13 and fig. 4.
Table 13 effective iodine 1% povidone-iodine solution at different dilutions to a bacterial concentration of 105cfu/ml E.coli, Staphylococcus aureusBacteriostatic results for staphylococci and Salmonella
Figure BDA0003082818290000181
Figure BDA0003082818290000191
The povidone iodine solution is diluted by adding water into 1 percent of effective iodine, has good killing effect on escherichia coli, salmonella and staphylococcus aureus, and the concentration of 4000 times of the diluted solution is 105Under the condition of cfu/ml, the killing rate reaches 100 percent.
And (eight) test: the invention relates to a moisturizing effect of povidone iodine solution
Povidone iodine solution for testing: the preparation method of the preparation is selected from the methods of examples 1 to 6.
Control group: iodine tincture
Test animals: selecting 70 rabbits with the same health condition and growth condition
Test design and method:
the test groups and the control groups were divided into 7 groups of 10 individuals by a random grouping method. Depilating two sides of rabbit back with 8% (mass percent) sodium sulfide, wherein the depilated area is about 150cm2The control group was smeared with 0.2mL of iodine tincture, the test group was smeared with 0.2mL of povidone-iodine solution diluted 10 times as prepared in examples 1 to 6, and the other feeding conditions were the same as those of the control group. Measuring stratum corneum water content of the part by capacitance method skin water content test probe at 15min, 30min, 60min, 90min, and 120 min. The test results are shown in Table 14.
Table 14 usage time and moisture content of skin stratum corneum test results (unit:%) of povidone-iodine solution according to the present invention
15min 30min 60min 90min 120min
Control group 54 45 43 39 40
Example 1 70 65 64 61 58
Example 2 68 62 60 54 50
Example 3 68 64 63 60 57
Example 4 71 67 65 62 60
Example 5 69 68 64 62 60
Example 6 70 68 66 64 60
As can be seen from Table 14, iodine tincture had a poor moisturizing effect, and the moisture content of the iodine tincture decreased to about 40% in a short time, whereas examples 1 to 6 all had good moisturizing effects, in which the moisture content of the horny layer of the skin was maintained at 50 to 60% or more.
Test nine: the invention relates to the dispersion condition of povidone iodine solution in water
Povidone iodine solution for testing: the preparation method of the compound is selected from the method of example 3.
Precisely measuring 0.5ml of povidone-iodine solution, dripping the povidone-iodine solution into 100ml of water, and observing the dissolution and dispersion conditions of the povidone-iodine solution in the water, wherein the test result is shown in fig. 5;
fig. 5 shows the dispersion condition of the povidone-iodine solution after standing and dissolving in water, the povidone-iodine solution is uniformly dispersed in water from top to bottom, the dispersibility is good, the dissolving speed is high, and the color in the cup is still dark reddish brown after several days. The invention relates to a povidone iodine solution which has the advantages of high dissolving speed in water, uniform dispersion, good stability, strong bactericidal power and good disinfection effect when being applied to aquatic product culture water body disinfection.
Test ten: the invention relates to application of povidone iodine solution in treating wounds of castrated piglets
Povidone iodine solution for testing: the preparation method of the preparation is selected from the methods of examples 1 to 6.
Test animals: 350 piglets in a certain pig farm with basically the same health condition.
Test design and method:
the test groups and the control groups were divided into 7 groups by a random grouping method, and each group had 50 heads. The control group was sprayed on post-castration wounds with iodine tincture, and the test groups were used as follows: diluting povidone iodine solution with water 10 times, mixing, spraying on wound after castration, and keeping the same feeding conditions as the control group.
The test period is 0-48 hours after castration, and the wound healing condition of the piglets is observed. The test results are shown in Table 15.
Watch 15
0 hour 24 hours healing status Healing at 48 hours
Control group The reaction of the piglets is severe The wound healed about 40%, and blood stain remained visible The wound healed about 52%, and a small amount of blood was still visible
Example 1 Mild, no too much stress reaction The wound heals about 64%, and has a small amount of blood stain The wound is approximately 88% healed and is substantially scabbed
Example 2 Mild, no too much stress reaction The wound heals about 68% with a small amount of blood The wound is about 91% healed and is basically scabbed
Example 3 Mild, no too much stress reaction The wound healed about 62%, with a small amount of blood The wound is approximately 90% healed and is substantially scabbed
Example 3 Mild, no too much stress reaction The wound is approximately 60% healed with a small amount of blood The wound heals about 86% and is basically scabbed
Example 4 Mild, no too much stress reaction The wound healed to about 67%, with a small amount of blood The wound is approximately 89% healed and is basically scabbed
Example 5 Mild, no too much stress reaction The wound is approximately 65% healed with a small amount of blood The wound is approximately 87% healed and is basically scabbed
Example 6 Mild, no too much stress reaction The wound heals about 68% with a small amount of blood The wound is approximately 90% healed and is substantially scabbed
As can be seen from table 15, the piglets obtained in application examples 1 to 6 had no stress reaction when compared with the control group using iodine tincture, the degree of healing of the wounds reached 60% or more after 24 hours, the wounds were substantially scabbed after 48 hours, the degree of healing reached 86% or more, and the degree of healing reached only 52% after 48 hours in the control group.
Test eleven: the invention relates to application of povidone iodine solution in treating cow mastitis
Povidone iodine solution for testing: the preparation method of the preparation is selected from the methods of examples 1 to 6.
Test animals: 175 cows with clinical mastitis in a certain pasture show the clinical symptoms: redness, edema, stiffness of affected breast areas, hard masses of varying size which may occur when palpating the breast, coagulated milk masses or purulent secretions in the curd.
Test design and method:
the test groups and the control groups were divided into 6 groups by a random grouping method, and each group had 25 heads. Iodine tincture was used for the control group, and the test group was used as follows: diluting the povidone iodine solution by 10 times with water, mixing uniformly, and carrying out medicated bath before and after milking in the milk area of the dairy cow suffering from mastitis respectively, wherein the rest feeding conditions are the same.
The test period is five days after the use, and the recovery condition of the cow breasts is observed.
The treatment principle of mastitis is as follows: after five days of administration, the symptoms of red, swollen, hot, painful and hard breasts disappear, no abnormal change is observed by naked eyes in milk, and the milk yield is recovered to be normal.
Effective judgment principle: after five days of administration, the symptoms of red, swollen, hot, painful and hard breasts, etc. are obviously relieved, the lump in the breast is obviously reduced, the milk property is basically normal, and the milk yield is not recovered.
An invalid judgment principle: after five days of administration, the symptoms of red, swollen, hot and painful breasts are not obviously relieved, and the breast milk is still clear and thin and has yellow color or is still abnormal by visual observation of flocculus, pus juice and the like.
The test results are shown in table 16 and fig. 6.
TABLE 16
Figure BDA0003082818290000221
Figure BDA0003082818290000231
It can be seen from table 16 and fig. 6 that the cured breasts of the control group are dry and dull, while the cured breasts of the cows using the test groups of examples 1-6 are full, bright and elastic, the total effective rate of the control group is 74.4% lower than that of the test groups, and the total effective rate of the test groups is more than 92.0%.
Test twelve: the invention relates to application of povidone iodine solution in treating chicks
Povidone iodine solution for testing: the preparation method is selected from the methods of examples 1, 3 and 6.
Test animals: 500 chicks in a certain farm with basically the same growth and health conditions
Test design and method:
the test groups and the control groups were divided into 4 groups of 100 individuals by a random grouping method. The control group used farm water and the test group used as follows: diluting povidone iodine solution with water by 5000 times, spraying to sterilize chicks and colony houses, and sterilizing with drinking water line, wherein the rest conditions are the same.
Continuously using the povidone iodine solution for 5 days, and observing and counting the survival rate and diarrhea rate of the chicks on the 15 th day after the use is finished.
The test results of the effect of povidone-iodine solution of the present invention on the survival rate and diarrhea rate of chicks are shown in table 17.
TABLE 17
Survival rate (%) Diarrhea Rate (%)
Control group 78 26
Example 1 88 12
Example 3 90 11
Example 6 89 9
It can be seen from table 17 that the survival rate of the control group directly using the water source of the farm is only 78%, the diarrhea rate is as high as 26%, the survival rate of the test composition applying the invention reaches 88% or more, and the diarrhea rate is 12% or less, thereby significantly improving the survival rate and reducing the diarrhea rate.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.

Claims (8)

1. The povidone-iodine solution is characterized by being prepared from the following components in parts by weight: 30-50 parts of povidone iodine, 30-40 parts of ethanol, 3-30 parts of water, 2-5 parts of potassium iodide, 2-4 parts of a stabilizer and 1.4-2.4 parts of a pH regulator.
2. The povidone-iodine solution of claim 1, wherein the stabilizing agent is hydroxypropyl methylcellulose.
3. The povidone-iodine solution of claim 1, wherein the hydroxypropylmethylcellulose has a viscosity of greater than 100 mPa-s.
4. The povidone-iodine solution of claim 1, wherein the pH modifier is sodium tripolyphosphate.
5. The povidone-iodine solution as defined in claim 4, wherein the sodium tripolyphosphate is present in an amount of 85.0% by weight or more, and the total phosphate is expressed as P2O5Counting: 56.0 wt% to 58.0 wt%.
6. The preparation method of the povidone-iodine solution is characterized by adopting the following components in parts by weight: 30-50 parts of povidone iodine, 30-40 parts of ethanol, 3-30 parts of water, 2-5 parts of potassium iodide, 2-4 parts of hydroxypropyl methyl cellulose and 1.4-2.4 parts of sodium tripolyphosphate; the preparation steps are as follows:
the method comprises the following steps: weighing potassium iodide and water according to the prescription amount, dissolving, and filling into a specific solution preparation container to form a body system 1;
step two: adding povidone iodine and ethanol with the prescribed amount into the system 1, placing an impeller of a dispersion machine at the center of a container, lowering the impeller to the lowest position, starting the machine to adjust the rotating speed to 1200r/min, and stirring for 30 minutes to form a system 2;
step three: adding hydroxypropyl methyl cellulose and sodium tripolyphosphate into the system 2, and stirring for 30 minutes to obtain the povidone-iodine solution.
7. The method of claim 6, wherein the special preparation vessel and the dispersing machine are made of metal materials, and the surface of the special preparation vessel and the dispersing machine is coated with Teflon.
8. The method of claim 6, wherein the specific preparation container has an inner barrel and an outer barrel, the inner barrel and the outer barrel are nested together, a coolant chamber is formed between the inner barrel and the outer barrel, and the coolant chamber has a coolant inlet and a coolant outlet.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012086760A1 (en) * 2010-12-24 2012-06-28 Meiji Seikaファルマ株式会社 Disinfectant
CN103202854A (en) * 2013-04-06 2013-07-17 江苏健裕健康医疗器械有限公司 Povidone iodine compound disinfectant
CN104013573A (en) * 2014-06-25 2014-09-03 山西神龙天翼科技有限公司 High-content liquid povidone-iodine
CN105853397A (en) * 2016-04-26 2016-08-17 上海宇昂新材料科技有限公司 Povidone iodine concentrated solution as well as preparation method and application thereof
CN108836951A (en) * 2018-06-20 2018-11-20 中山万汉制药有限公司 A kind of povidone iodine slow-release medicine-membrane and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012086760A1 (en) * 2010-12-24 2012-06-28 Meiji Seikaファルマ株式会社 Disinfectant
CN103202854A (en) * 2013-04-06 2013-07-17 江苏健裕健康医疗器械有限公司 Povidone iodine compound disinfectant
CN104013573A (en) * 2014-06-25 2014-09-03 山西神龙天翼科技有限公司 High-content liquid povidone-iodine
CN105853397A (en) * 2016-04-26 2016-08-17 上海宇昂新材料科技有限公司 Povidone iodine concentrated solution as well as preparation method and application thereof
CN108836951A (en) * 2018-06-20 2018-11-20 中山万汉制药有限公司 A kind of povidone iodine slow-release medicine-membrane and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
巴剑波等: "聚维酮碘溶液消毒性能观察", 《中国消毒学杂志》 *

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