CN107028977B - Ozonized oil complex and preparation method and application thereof - Google Patents

Ozonized oil complex and preparation method and application thereof Download PDF

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CN107028977B
CN107028977B CN201611010322.XA CN201611010322A CN107028977B CN 107028977 B CN107028977 B CN 107028977B CN 201611010322 A CN201611010322 A CN 201611010322A CN 107028977 B CN107028977 B CN 107028977B
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ozonized oil
parts
stirring
ozone
preparation
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CN107028977A (en
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陈耕
李宜炀
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HUBEI JINGGENG BIOLOGICAL ENGINEERING CO., LTD.
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Hubei Jinggeng Bioengineering Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients

Abstract

The invention provides an ozonized oil complex and a preparation method and application thereof. According to the invention, under the vacuum closed condition, 50-120 parts by mass of ozonized oil, 30-80 parts by mass of cream matrix and 10-20 parts by mass of water are mixed and kept stand at 10-15 ℃ to obtain the ozonized oil complex. The preparation method provided by the invention has low cost, and the ozone content is deep into the matrix molecules to form the ozonized oil complex with a closed and steady structural state, so that the technical defect of quick release of ozone molecules due to high temperature is overcome, and the slow release effect is achieved.

Description

Ozonized oil complex and preparation method and application thereof
Technical Field
The invention relates to the technical field of medical materials, in particular to an ozonized oil complex and a preparation method and application thereof.
Background
Ozone has strong oxidation effect, ozone molecules can directly act on membrane proteins on the surfaces of bacteria and viruses to denature the bacteria and the viruses, and further, DNA and RNA of the bacteria and the viruses are damaged and cannot be copied, so that the sterilization effect is achieved. Because ozone has a killing effect on various bacteria propagules, spores, viruses, herpes, molds, protozoa and the like, high-concentration oxygen generated in the ozone decomposition process can promote granulation growth and repair of damaged tissues, so that the ozone plays an important role in the field of medicine. At present, the domestic market only prepares ozone through an ozone generator and is clinically applied to the treatment of gynecological inflammation.
Ozone, a very unstable gas, can be combined by unsaturated fatty vegetable oils into a stable ozonide, i.e. an ozonized oil. Currently, most of the ozonized oil is ozonized saturated by injecting ozone into sunflower oil, olive oil or edible oil for about two days until the oil becomes solid. When the ozonized oil is coated on the exudate of the wound surface, the ozonized oil reacts with the biological molecules to generate and release stable hydrogen peroxide. The disinfection and improved oxidation may accelerate scar formation. The ozonized oil can be used for preventing and treating bacterial and fungal dermatosis, surgical infection, anal inflammation, gynecological inflammation, acne, dental caries, gingivitis, stomatitis, etc., has bactericidal effect on staphylococcus aureus, escherichia coli, candida albicans (mold), trichomonad, etc., and the redundant ozone is decomposed into nontoxic oxygen, has no residue, drug resistance and side effect.
However, the molecular structure of ozone in the ozonized oil is stable only in a low-temperature state, so that the ozonized oil is not easy to volatilize, the molecular structure of ozone is unstable and volatile due to high temperature, and the ozonized oil product popular in the market needs to be stored at low temperature, so that the use and popularization of the ozone technology are greatly reduced. While the prior art has patents on ozonized oil, such as Chinese patent CN102178632A, which discloses the application of ozonized oil in the preparation of raw materials for medical and health care products, the patent prepares ozonized oil products by simple stirring, but the simple stirring can not stabilize the molecular structure of ozone, so the technologies can not solve the problem that the ozonized oil needs to be stored at low temperature.
Disclosure of Invention
The invention aims to provide an ozonized oil complex and a preparation method and application thereof. The preparation method provided by the invention has low cost, and the prepared ozonized oil complex has a stable structure and does not need low-temperature storage.
The invention provides a preparation method of an ozonized oil complex, which comprises the following steps:
under the vacuum sealing condition, 50-120 parts by mass of ozonized oil, 30-80 parts by mass of cream matrix and 10-20 parts by mass of water are mixed and kept stand at 10-15 ℃ to obtain the ozonized oil complex.
Preferably, the cream base is expanded prior to mixing.
Preferably, the mixing is performed under stirring conditions, and the stirring includes clockwise stirring and counterclockwise stirring.
Preferably, the standing time is 12-20 h.
Preferably, the standing still further comprises: and cooling the standing material to 0-5 ℃, stirring, and then heating to 30-38 ℃.
Preferably, the cooling rate is 1-5 ℃/h.
Preferably, the stirring speed is 800-1200 r/min, and the stirring time is 4-8 h.
Preferably, the temperature rising rate is 10-20 ℃/h.
The invention also provides the ozonized oil complex prepared by the preparation method in the technical scheme, wherein the mass concentration of ozone in the ozonized oil complex is 10-85%.
The invention also provides the application of the ozonized oil complex in the technical scheme in medical health care products.
According to the invention, under the vacuum closed condition, 50-120 parts by mass of ozonized oil, 30-80 parts by mass of cream matrix and 10-20 parts by mass of water are mixed and kept stand at 10-15 ℃ to obtain the ozonized oil complex. The preparation method provided by the invention has low cost, and the ozonized oil complex with a closed and steady structural state is formed by leading the ozone content to be deep into the molecules of the cream matrix, thereby solving the technical defect of quick release of ozone molecules caused by high temperature and achieving the slow release effect.
Detailed Description
The invention provides a preparation method of an ozonized oil complex, which comprises the following steps: under the vacuum sealing condition, 50-120 parts by mass of ozonized oil, 30-80 parts by mass of cream matrix and 10-20 parts by mass of water are mixed and kept stand at 10-15 ℃ to obtain the ozonized oil complex.
The ozonized oil complex provided by the invention comprises 50-120 parts of ozonized oil, preferably 70-100 parts of ozonized oil, and more preferably 80-90 parts of ozonized oil complex. In the present invention, the ozonized oil is preferably sunflower oil trioxide. The type of the ozonized oil used in the present invention is not particularly limited, and commercially available ozonized oil known to those skilled in the art may be used.
The ozonized oil complex provided by the invention comprises 30-80 parts of cream matrix, preferably 40-70 parts of cream matrix, and more preferably 50-60 parts of cream matrix. The kind of the cream base is not particularly limited in the present invention, and cream bases well known to those skilled in the art may be used. In the present invention, the cream base is preferably a medical grade gel, cream or cream, more preferably one or more of carbomer, carboxymethylcellulose, stearic acid and petrolatum. In the present invention, the cream base absorbs ozone from the complexed ozonized oil, forming a stable structure.
The ozonized oil complex provided by the invention comprises 10-20 parts of water, preferably 13-17 parts of water. In the invention, the water can increase the solubility of the ozonized oil in the matrix, dilute the materials and facilitate stirring and complexing.
In the present invention, the cream base is preferably subjected to a swelling treatment before mixing. In the present invention, the puffing treatment is preferably: the cream base is soaked in water. In the present invention, the amount of water in the expansion process is preferably such that it covers the cream base. In the invention, the time of the puffing treatment is preferably 44-50 h, and more preferably 46-48 h.
The ozonized oil complex is prepared by mixing ozonized oil, cream matrix and water under a vacuum closed condition, and standing at 10-15 ℃. In the present invention, the preparation of the ozonized oil complex is preferably performed under vacuum closed aseptic conditions. In the present invention, the degree of vacuum of the vacuum is preferably 28 to 32 Pa. The present invention is not particularly limited to the ozonized oil complex production apparatus, and an apparatus capable of providing a vacuum-tight space, which is well known to those skilled in the art, may be used. In the present invention, the ozonated oil complex is preferably carried out in a bioreactor.
In the present invention, the mixing is preferably performed under stirring conditions. In the invention, the stirring speed is preferably 900-1000 r/min, and the stirring time is preferably 40-60 min.
In the present invention, the stirring includes clockwise stirring and counterclockwise stirring. In the present invention, the stirring is preferably performed by stirring clockwise and then anticlockwise, or by stirring counterclockwise and then stirring clockwise. In the invention, the speed of clockwise stirring is preferably 900-1000 r/min, and the time of clockwise stirring is preferably 20-30 min; the speed of the anticlockwise stirring is preferably 900-1000 r/min, and the time of the anticlockwise stirring is preferably 20-30 min. In the present invention, the stirring is performed to sufficiently mix the components uniformly.
After mixing, the obtained mixed material is kept stand at the temperature of 10-15 ℃ to obtain the ozone oil complex. In the invention, the temperature of the standing is preferably 12-14 ℃; the standing time is preferably 12-20 h, more preferably 14-18 h, and most preferably 15-17 h. In the present invention, the ozonized oil is sufficiently miscible with the cream base during said resting, to form a stable complex of ozone in the base. In the present invention, the temperature of the resting may reduce the rate at which ozone is volatilized into a gas, complexing the ozone with the cream base.
After the standing is finished, the invention preferably observes the surface of the material to judge the degree of the complex reaction and judges whether the complex reaction is complete. Specifically, if the surface of the material has no oil droplets, the complexing reaction is sufficient; when oil droplets exist on the surface of the material, the complexing reaction is insufficient, and the material is preferably heated to 16-20 ℃ for secondary standing. The time of the secondary standing is not specially limited, and the secondary standing is only needed when the surface of the material has no oil droplets. In the invention, the time for the secondary standing is preferably 4-12 h, and more preferably 6-10 h.
According to the invention, preferably, after no oil drop exists on the surface of the material, the temperature is reduced to 0-5 ℃, stirring is carried out, and then the temperature is increased to 30-38 ℃, so that the ozonized oil complex is obtained. In the invention, the cooling rate is preferably 1-5 ℃/h, and more preferably 3-4 ℃. In the invention, the temperature reduction can make the volatilized ozone return to a liquid state again along with the temperature reduction and dissolve in the cream matrix, thereby facilitating further complexation.
In the invention, the stirring speed after cooling is preferably 800-1200 r/min, and more preferably 900-1100 r/min; the stirring time is preferably 4-8 h, and more preferably 5-7 h. In the present invention, ozone is further complexed in the cream base during the stirring process, forming a stable structure.
In the invention, the temperature rise is further preferably 33-35 ℃; the heating rate is preferably 10-20 ℃/h, and more preferably 12-16 ℃/h. In the present invention, at the rate of temperature increase, ozone molecules that do not complex to form stable structures are rapidly volatilized from the matrix.
The invention preferably repeats the steps of cooling, stirring, heating and secondary standing to achieve the purpose that the surface of the material has no oil droplets.
The invention also provides the ozonized oil complex prepared by the preparation method in the technical scheme, wherein the mass concentration of ozone in the ozonized oil complex is 10-85%, preferably 40-80%, and more preferably 60-70%.
The invention also provides the application of the ozonized oil complex in the technical scheme in medical health care products. In the present invention, the substance is preferably a bactericide; in use, the ozonated oil complex is preferably applied directly to the skin surface or applied to the skin surface in a carrier material.
To further illustrate the present invention, the ozonized oil complex provided by the present invention and the preparation method and application thereof are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1:
adding 80 parts of carbomer, adding equivalent amount of water, puffing for 48h, mixing with 120 parts of ozonized oil and 20 parts of water in a biological reaction kettle, stirring to uniformly mix the components, and standing at 15 ℃ for 20h to obtain the ozonized oil complex.
The ozonized oil complex prepared by the embodiment has the mass concentration of ozone of 10 percent, can be stored at normal temperature, and reduces the ozone amount by 2 percent after being stored for 360 days at normal temperature.
Example 2:
the ozonized oil complex obtained in example 1 is used as blue-oxygen gel for vaginal packing, is used for killing various bacteria, mold and trichomonad, and is applied to skin surface for accelerating sterilization.
Example 3:
30 parts of carboxymethyl cellulose and 10 parts of medical polyvinyl alcohol, adding equivalent water, puffing for 48 hours, mixing with 120 parts of ozonized oil and 20 parts of water in a biological reaction kettle, stirring clockwise for 30 minutes, stirring anticlockwise for 30 minutes, and standing at 15 ℃ for 10 hours;
cooling to 2 deg.C at 3 deg.C/h rate, stirring at 1000r/min for 6h, and heating to 35 deg.C at 10 deg.C/min rate to obtain ozonized oil complex.
The ozonized oil complex prepared by the embodiment has the ozone mass concentration of 80 percent, can be stored at normal temperature, and reduces the ozone amount by 2 percent after being stored for 360 days at normal temperature.
Example 4:
the ozonized oil complex obtained in the example 3 is coated in non-woven fabric to be made into a patch, and the patch is packaged in a sealed inner packaging material and applied to skin sterilization, beauty treatment and sterilization without low-temperature storage at normal temperature.
Example 5:
80 parts of stearic acid, equivalent water is added for puffing for 48 hours, and the stearic acid, 120 parts of ozonized oil and 20 parts of water are mixed in a biological reaction kettle, stirred clockwise for 30 minutes, stirred anticlockwise for 30 minutes and kept stand for 10 hours at 15 ℃;
cooling to 2 deg.C at 3 deg.C/h rate, stirring at 1000r/min for 6h, and heating to 35 deg.C at 10 deg.C/min rate to obtain ozonized oil complex.
The ozonized oil complex prepared by the embodiment has the mass concentration of ozone of 40 percent, can be stored at normal temperature, and reduces the ozone amount by 2 percent after being stored for 360 days at normal temperature.
Example 6:
mixing 60 parts of vaseline, 120 parts of ozonized oil and 20 parts of water in a biological reaction kettle, stirring to uniformly mix the components, clockwise stirring for 30min, anticlockwise stirring for 30min, and standing for 10h at 15 ℃; cooling to 2 deg.C at 3 deg.C/h rate, stirring at 1000r/min for 6h, and heating to 35 deg.C at 10 deg.C/min rate to obtain ozonized oil complex.
The ozonized oil complex prepared by the embodiment has the mass concentration of ozone of 20 percent, can be stored at normal temperature, and reduces the ozone amount by 2 percent after being stored for 360 days at normal temperature.
Comparative example 1:
adding 80 parts of carbomer, adding equivalent water, puffing for 48 hours, mixing with 120 parts of ozonized oil and 20 parts of water in a biological reaction kettle, and stirring at the normal temperature at the speed of 6000r/min for 4 hours to uniformly mix all the components to obtain the ozonized oil product.
The products of comparative example 1 and example 1 were subjected to oxygen content emission rate tests under normal temperature non-closed and closed conditions, and the results are shown in tables 1 and 2, respectively. As can be seen from tables 1 and 2, the preparation method provided by the invention can enable ozone to form a stable complex, reduce the diffusion speed under normal temperature and pressure and closed conditions, and improve the slow release property.
TABLE 1 comparison of oxygen evolution rates for comparative example 1 and example 1 under ambient temperature non-closed conditions
Figure BDA0001154777070000061
TABLE 2 comparison of oxygen evolution rates for comparative example 1 and example 1 under ambient temperature sealing conditions
Figure BDA0001154777070000062
As can be seen from the above examples, the ozonized oil complex prepared by the preparation method provided by the invention has low oxygen diffusion speed at normal temperature and does not need low-temperature storage.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (8)

1. A method of preparing an ozonated oil complex, comprising the steps of:
under the vacuum closed condition, 50-120 parts of ozonized oil, 30-80 parts of cream matrix and 10-20 parts of water are mixed in parts by mass, the mixture is stood at 10-15 ℃, the stood material is cooled to 0-5 ℃ for stirring, then the temperature is raised to 30-38 ℃, the steps of cooling, stirring, heating and standing are repeated, the surface of the material is free of oil droplets, and an ozonized oil complex is obtained, wherein the mass concentration of ozone in the ozonized oil complex is 20-40%.
2. The method of claim 1, wherein the cream base is expanded prior to mixing.
3. The method of claim 1, wherein the mixing is performed under agitation conditions, the agitation including clockwise agitation and counterclockwise agitation.
4. The preparation method according to claim 1, wherein the standing time is 12-20 h.
5. The preparation method according to claim 1, wherein the cooling rate is 1-5 ℃/h.
6. The preparation method of claim 1, wherein the stirring speed is 800-1200 r/min, and the stirring time is 4-8 h.
7. The preparation method according to claim 1, wherein the temperature rise rate is 10 to 20 ℃/h.
8. The ozonized oil complex produced by the production method according to any one of claims 1 to 7, wherein the mass concentration of ozone in the ozonized oil complex is 20 to 40%.
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CN109528754A (en) * 2019-01-17 2019-03-29 余浚龙 Composition, externally applied drug, preparation method and its application for treating the externally applied drug of inner cavity mucosal inflammation
CN109876007B (en) * 2019-04-12 2021-07-16 重庆渠济生物科技有限公司 Ozone antibacterial and disinfecting gel and preparation method thereof
CN110786994B (en) * 2019-10-24 2022-05-20 万明 Double-component active oxygen bacteriostatic sanitary towel and preparation method thereof

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WO2007046122A2 (en) * 2005-10-17 2007-04-26 Bioo3Pharma S.R.L. Ozonised oil, process for the preparation and use thereof in medical field
CN101342240A (en) * 2008-07-17 2009-01-14 岳泉 Externally used medical ointment for treating dermatosis, uses, preparation method and apparatus thereof
CN102178632A (en) * 2011-05-06 2011-09-14 石平安 Application of ozonized oil to preparation of raw materials of medical health-care products
CN103430797A (en) * 2013-08-13 2013-12-11 陕西省微生物研究所 Method for preventing and controlling fungal diseases of cucumbers
CN105769907A (en) * 2016-03-08 2016-07-20 邓育德 Effective antifungal complex and preparing method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007046122A2 (en) * 2005-10-17 2007-04-26 Bioo3Pharma S.R.L. Ozonised oil, process for the preparation and use thereof in medical field
CN101342240A (en) * 2008-07-17 2009-01-14 岳泉 Externally used medical ointment for treating dermatosis, uses, preparation method and apparatus thereof
CN102178632A (en) * 2011-05-06 2011-09-14 石平安 Application of ozonized oil to preparation of raw materials of medical health-care products
CN103430797A (en) * 2013-08-13 2013-12-11 陕西省微生物研究所 Method for preventing and controlling fungal diseases of cucumbers
CN105769907A (en) * 2016-03-08 2016-07-20 邓育德 Effective antifungal complex and preparing method thereof

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