CN102274177A - Compound thymol nanometer medicament and preparation method thereof - Google Patents
Compound thymol nanometer medicament and preparation method thereof Download PDFInfo
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- CN102274177A CN102274177A CN2011102430532A CN201110243053A CN102274177A CN 102274177 A CN102274177 A CN 102274177A CN 2011102430532 A CN2011102430532 A CN 2011102430532A CN 201110243053 A CN201110243053 A CN 201110243053A CN 102274177 A CN102274177 A CN 102274177A
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Abstract
The invention discloses a compound thymol nanometer medicament. The grain diameter of the medicament is between 1 and 100 nanometers, and the medicament consists of the following raw materials in percentage by mass: 0.1 to 9 percent of thymol, 0.1 to 9 percent of eugenol, 0.2 to 6 percent of oil phase, 20 to 40 percent of surfactant, 4 to 20 percent of cosurfactant and the balance of distilled water, wherein the sum of the mass percentage of the raw materials is 100 percent. By the medicament, the effects of antibiosis, inflammation relieving, desinsection, desinsectization and the like of the original thymol greatly are improved greatly; and the medicament belongs plant source medicaments, does not have residues of food and meat medicaments and cause the tolerance of pathogeny, so the medicament is an efficient and safe nanometer medicament for resisting dermatozoon.
Description
Technical field
The invention belongs to field of medicaments, relate to a kind of compound medicine novel form, particularly a kind of preparation method of compound recipe thymol Nano medication of stable transparent.
Background technology
Thymol separates from hundred li grass at first and obtains and gain the name.Its English name is " thymol ", and the thymol chemical name is 3-methyl-6-isopropyl-phenol.Room temperature is insoluble in water for white to light yellow crystalline powder down, easy and immiscible organic solvent, 233 ℃ of boiling points, 48 ~ 51 ℃ of fusing points.
Thymol has hundred li grass or thymy special aroma, has anti-corrosive properties, and toxicity is lower than phenol, has medical value, can be used in the dental health article; It also has antifungal and parasite function, can be used to handle wound, stores dissec etc.; Because it has the phenols abnormal smells from the patient, also is usually used in anthelmintic, has the strong parasitic effects such as removing acarid of killing.
Eugenol is 4-pi-allyl-2-methoxyphenol, is the dulcet chemical compound of a kind of oily, is the effective ingredient in a lot of Chinese herbal medicine such as Flos Caryophylli, the Cortex Cinnamomi, and is water-soluble hardly, with ethanol, ether and wet goods can be miscible.The eugenol wide material sources are easy to preparation, are a kind of good plant source medicines, and pharmacological action is widely arranged.
More than two kinds of medicine dissolutions relatively poor, physical instability.The medicine for the treatment of dermatozoiasis in the market mostly is ivermectin, and its life cycle is longer, and is bigger for the house pet toxic and side effects, and effect is not remarkable.
Summary of the invention
At the shortcomings and deficiencies that exist in the prior art, the present invention makes up thymol and eugenol, and purpose is to provide that a kind of dissolubility is good, physical property is stable, safe and effective compound recipe thymol Nano medication.
The technical method of realizing the foregoing invention purpose is a compound recipe thymol Nano medication, and it is made up of the raw material of following mass percent:
Thymol 0.1%～9%, eugenol 0.1%～9%, oil phase 0.2%～6%, surfactant 20%～40%, cosurfactant 4%～20%, surplus are distilled water, and the mass percent sum of above-mentioned raw materials is 100%.
The formula optimization mass percent scope of preparation medicine of the present invention is: thymol 0.5%～5%, eugenol 0.5%～5%, oil phase 0.5%～4%, surfactant 25%～35%, cosurfactant 4.5%～10%, surplus are distilled water, and the mass percent sum of above-mentioned raw materials is 100%.
The prescription best in quality percentage ratio of preparation medicine of the present invention is: thymol 2%, eugenol 2%, oil phase 1%, surfactant are 30%, cosurfactant is 5%, distilled water 60%.
Described surfactant is one or more the mixture in tween 80 (Tween-80), Tween-60 (Tween-60), tween 20 (Tween-20), polyoxyethylene (40) castor oil hydrogenated (RH-40), polyoxyethylene (40) Oleum Ricini (EL-40) and the Arlacel-80 (Span-80).
Described cosurfactant is dehydrated alcohol, ethylene glycol, 1, the mixture of one or more in 2-propylene glycol, glycerol, Macrogol 200 (PEG 200), PEG400 (PEG 400), the Macrogol 600 (PEG 600).
Described oil phase is one or more the mixture in oleic acid, ethyl oleate, isopropyl myristate, liquid paraffin, vitamin E oil, Jojoba oil, triacetyl glycerine, ethyl acetate, almond oil, glycerin methylal, Semen Tritici aestivi germ oil, olive oil, the Oleum Ricini.
In the selection of surfactant, the present invention selects the nonionic surfactant of avirulence and good biocompatibility for use.Nonionic surfactant is more stable in solution, is not subject to the influence of strong electrolyte, inorganic salts, also is not subject to the influence of soda acid, and good with the compatibility of other surfactants, haemolysis is less.In theory, the preparation of O/W type nanometer emulsion needs the HLB value of surfactant between 8～18, consider preparation technology's simplicity, be the easy formation of nano-emulsion and the stability of nano-emulsion, the present invention selects the liquid nonionic surfactant of HLB between 10～15 for use, and is perhaps composite with the nonionic surfactant of a kind of HLB＜10.Available surfactant has: the mixture of one or more among Tween-80, Tween-60, Tween-20, RH-40, EL-40 and the Span-80.
The present invention is according to when the HLB value of the required surfactant of emulsifying oil phase is close with surfactant, the principle that formed emulsion is stable, the oils and fats of selecting for use has: the mixture of one or more in oleic acid, ethyl oleate, isopropyl myristate, liquid paraffin, vitamin E oil, Jojoba oil, triacetyl glycerine, ethyl acetate, almond oil, glycerin methylal, Semen Tritici aestivi germ oil, olive oil, the Oleum Ricini.
The formation of most of nano-emulsion all needs to add cosurfactant, and its effect mainly contains: reduce interfacial tension between profit, the flowability that increases interfacial film, the HLB value of reconciliation statement surface-active agent etc.The cosurfactant that the present invention selects for use has: dehydrated alcohol, ethylene glycol, 1, the mixture of one or more among 2-propylene glycol, glycerol, PEG 200, PEG 400, the PEG 600.
The present invention goes back the preparation method that a purpose provides above-mentioned compound recipe thymol Nano medication, specifically comprises the following steps:
1) take by weighing thymol, eugenol, oil phase, surfactant, cosurfactant, distilled water, standby;
2) thymol and eugenol are added in the oil phase, stir;
3) with step 2) solution of preparation adds to stir in the cosurfactant that it is dissolved fully, surfactant is added wherein again, stir;
4) solution with the step 3) preparation fully stirs at 20 ℃～25 ℃ slow down adding distilled water, has mobile yellow or water white compound recipe thymol Nano medication for a short time until formation clear, viscosity.
The principle of compound recipe thymol Nano medication option table surface-active agent phase of the present invention and oil phase:
1) preparation of surfactant phase: composite as need, then calculate the HLB value of system behind two kinds of surfactant compounds.Because the HLB value of surfactant has additive properties, the available quality averaging method is obtained the HLB value of surfactant.For example, after two kinds of surfactant A, B mix, the hydrophile-lipophile balance HLB of its mixed surfactant
ABValue is
HLB
AB=（W
AHLB
A+W
BHLB
B）/(W
A+W
B)
W in the formula
A, W
BThe quality of-blend surfactants A, B;
HLB
A, HLB
BThe HLB value of-surfactant A, B.
2) preparation of oil phase is selected one or more oil according to the HLB value of surfactant phase, transfers its ratio, makes the required HLB value of its emulsifying close with surfactant HLB value mutually.
Compound recipe thymol Nano medication of the present invention has the function of treatment dermatozoiasis.Usage: be coated with every day 1～2 time, continuous 1～2 week outside local.
The present invention detects through transmission electron microscope, and droplet diameter distribution is between 1nm～100nm, and outward appearance is yellow or colourless transparent liquid, has good stability:
1. light stability
Compound recipe thymol Nano medication is packed in the vial, and sealing places room temperature, and illumination 10d is in 1d, 3d, 5d, 7d, the 10d detection of taking a sample.The result shows that compound recipe thymol Nano medication outward appearance is clear still, does not have phenomenons such as muddiness, layering, precipitation, and particle diameter remains between 1nm ~ 100nm.
2. temperature stability
An amount of compound recipe thymol Nano medication is packed in the vial, and sealing places 4 ℃ respectively, keeps sample under 25 ℃ and 37 ℃ of three kinds of temperature conditions and investigates 30d, every 5d sampling observation.The result shows that this compound recipe thymol Nano medication all keeps clear under these three kinds of temperature conditions, do not see layering, muddiness and sedimentary phenomenon.
3. anti-freeze-stable
Compound recipe thymol Nano medication in-4 ℃ of one weeks of preservation, is returned to room temperature after the taking-up.This compound recipe thymol Nano medication becomes solid in the time of-4 ℃, return to after the room temperature it and return to transparently, and places after a week still clear.
4. accelerated stability
Compound recipe thymol Nano medication is placed centrifuge tube, and in the centrifugal 20min of 15000rpm, observed result is found its not layering, still clear.
Compound recipe thymol Nano medication of the present invention compared with prior art has the following advantages:
1) thermodynamic stability is good, the bin stability height, put for a long time not stratified, through centrifugal acceleration test layering not yet;
2) the invention belongs to nano-grade medicine, the outward appearance clear, the emulsion droplet dispersion is good, the bioavailability height;
3) medicine of the present invention can be treated dermatozoiasis safely and effectively.
4) preparation technology is simple, is fit to large-scale production.
Description of drawings
Fig. 1 is the transmission electron microscope picture of compound recipe thymol Nano medication of the present invention.
The specific embodiment
Below by the beneficial effect of the further elaboration of test example medicine of the present invention, these test examples comprise transmission electron microscope observation test, the test of stripped demodicid mite extremely and the clinical efficacy test of medicine of the present invention.
Test example 1Compound recipe thymol Nano medication transmission electron microscopy observation
Medicine of the present invention carries out microscopic pattern with transmission electron microscope to be observed, Fig. 1 is seen in result's demonstration, Fig. 1 is a compound recipe thymol Nano medication transmission electron microscope photo, show compound recipe thymol Nano medication drip spherical in shape and be evenly distributed, decentralized is good, particle diameter is all less than 100nm.
Test example 2Compound recipe thymol Nano medication exsomatizes and kills the demodicid mite test
Scrape the crust and the epidermis affected part scurf that cover with blood crusts in the rabbit auditory meatus of taking from right infection acarid, and place in the glass dish with the tweezers taking-up, the plate edge is coated with a small amount of acarid repellent agent, heats a little, is for experiment with choosing the active strong acarid of worm pin picking.
With separating pin picking acarid on the spill microscope slide, drip for two of reagents, 8 of the acarids of selecting are placed medicinal liquid and add coverslip, under inverted microscope, continue to observe 24h, observe once every 5min, each observation 2min that continues observes until all death of 8 acarids, record acarid death time every group.It is 3 groups that test is divided into, and all the other two groups is distilled water test group and ivermectin injection group, and test method is with compound recipe thymol Nano medication group.
Result of the test: different medicinal liquids are handled 24h result and are shown that it is 2 ~ 3min that compound recipe thymol Nano medication kills the demodicid mite time, is lower than the ivermectin injection group, and its miticidal effect is better than ivermectin injection.The results are shown in Table 1.
The table 1 miticidal effect comparative result that exsomatizes
Annotate :+expression has the acarid survival;-expression acarid all kills does not have recovery
Test example 3The test of compound recipe thymol Nano medication clinical efficacy
At hospital admission, make a definite diagnosis the trouble malis through check; After obtaining owner and agreeing, meet several 40 of the house pet of this experimental condition, as this object of study.Trial drug directly is applied to the affected part, and 14 d, are used continuously at every day twice in cleaning and dry affected part before the medication.The observed and recorded result of the test.
The effective percentage of table 2 medicine
The clinical efficacy result of the test shows, compound recipe thymol Nano medication effective percentage is 95%, and the effective percentage of clinical commonly used drug ivermectin is 90%, the clinical therapeutic efficacy that compound recipe thymol Nano medication is described is better than ivermectin, and safety, untoward reaction is few, has broad prospect of application aspect the treatment of dermatozoiasis.
Below the embodiment that provides by the inventor further set forth the preparation method of compound recipe thymol Nano medication of the present invention.
Embodiment 1
The preparation method of compound recipe thymol Nano medication of the present invention specifically comprises the following steps:
1) thymol 0.25g and eugenol 0.25g are added in the mixture of isopropyl myristate 0.02g and Jojoba oil 0.02g, stir;
2) solution with the step 1) preparation adds dehydrated alcohol 0.5g and 1, stirs in the mixture of 2-propylene glycol 0.3g it is dissolved fully, RH-40 3g is added again, and stirs;
3) with step 2) solution of preparation adds down slowly distilled water at 20 ℃～25 ℃ and fully stirs, until form clear, viscosity has mobile yellow or water white compound recipe thymol Nano medication for a short time.
Embodiment 2
Thymol 0.20g, eugenol 0.15g, isopropyl myristate 0.02g, Jojoba oil 0.02g, RH-40 3g, dehydrated alcohol 0.4g, 1,2-propylene glycol 0.3g, distilled water 5.91g.
Embodiment 3
Thymol 0.05g, eugenol 0.05g, ethyl acetate 0.1g, almond oil 0.1g, Tween-80 3g, Tween-20 0.5g, dehydrated alcohol 0.25g, ethylene glycol 0.25g, distilled water 5.7g.
Embodiment 4
Thymol 0.9g, eugenol 0.1g, olive oil 0.05g, Oleum Ricini 0.05g, Tween-80 3.5g, Tween-60 0.5g, dehydrated alcohol 0.5g, glycerol 0.5g, distilled water 3.9g.
Embodiment 5
Thymol 0.01g, eugenol 0.01g, ethyl acetate 0.6g, EL-40 3.5g, dehydrated alcohol 0.4g, PEG400 0.1g, distilled water 5.38g.
Embodiment 6
Thymol 0.2g, eugenol 0.2g, ethyl acetate 0.1g, Tween-80 3g, dehydrated alcohol 0.5g, distilled water 6g.
Embodiment 7
Thymol 0.1g, eugenol 0.1g, vitamin E oil 0.1 g, Semen Tritici aestivi germ oil 0.1 g, RH-40 3g, dehydrated alcohol 2g, distilled water 4.6g.
Embodiment 8
Thymol 0.05g, eugenol 0.05g, oleic acid 0.05g, liquid paraffin 0.05g, Tween-80 2g, dehydrated alcohol 0.8g, distilled water 7g.
Embodiment 9
Thymol 0.3g, eugenol 0.1g, glycerin methylal 0.01g, triacetyl glycerine 0.01g, Tween-80 3g, PEG600 0.2g, PEG200 0.2g, distilled water 6.18g.
Embodiment 10
Thymol 0.1g, eugenol 0.9g, isopropyl myristate 0.1g, Tween-80 3g, Span-80 0.5g, dehydrated alcohol 0.5g, distilled water 4.9g.
Embodiment 11
Thymol 0.1g, eugenol 0.1g, ethyl oleate 0.1g, EL-40 3g, dehydrated alcohol 0.5g, distilled water 6.2g.
Claims (9)
1. compound recipe thymol Nano medication, it is characterized in that, the particle diameter of this medicine is between 1nm～100nm, raw material by following mass percent is formed: thymol 0.1%～9%, eugenol 0.1%～9%, oil phase 0.2%～6%, surfactant 20%～40%, cosurfactant 4%～20%, surplus are distilled water, and the mass percent sum of above-mentioned raw materials is 100%;
Described surfactant is one or more the mixture among Tween-80, Tween-60, Tween-20, RH-40, EL-40 and the Span-80;
Described cosurfactant is dehydrated alcohol, ethylene glycol, 1, the mixture of one or more among 2-propylene glycol, glycerol, PEG 200, PEG 400, the PEG 600;
Described oil phase is one or more the mixture in oleic acid, ethyl oleate, isopropyl myristate, liquid paraffin, vitamin E oil, Jojoba oil, triacetyl glycerine, ethyl acetate, almond oil, glycerin methylal, Semen Tritici aestivi germ oil, olive oil, the Oleum Ricini.
2. compound recipe thymol Nano medication according to claim 1 is characterized in that, is made up of the raw material of following mass percent:
Thymol 0.5%～5%, eugenol 0.5%～5%, oil phase 0.5%～4%, surfactant are 25%～35%, cosurfactant is 4.5%～10%, surplus is a distilled water, and the mass percent sum of above-mentioned raw materials is 100%.
3. compound recipe thymol Nano medication according to claim 1 is characterized in that, is made up of the raw material of following mass percent:
Thymol 2%, eugenol 2%, oil phase 1%, surfactant are 30%, cosurfactant is 5%, distilled water 60%.
4. a compound recipe thymol Nano medication is characterized in that, is made up of the raw material of following mass percent:
Thymol 2.5%, eugenol 2.5%, isopropyl myristate 0.2%, Jojoba oil 0.2%, RH-40 30%, dehydrated alcohol 5%, 1,2-propylene glycol 3%, distilled water 56.6%.
5. a compound recipe thymol Nano medication is characterized in that, is made up of the raw material of following mass percent:
Thymol 0.5%, eugenol 0.5%, ethyl acetate 1 %, almond oil 1 %, Tween-80 30%, Tween-20 5 %, dehydrated alcohol 2.5%, ethylene glycol 2.5 %, distilled water 57%.
6. a compound recipe thymol Nano medication is characterized in that, is made up of the raw material of following mass percent:
Thymol 1%, eugenol 1%, ethyl oleate 1%, EL-40 30%, dehydrated alcohol 5%, distilled water 62%.
7. a compound recipe thymol Nano medication is characterized in that, is made up of the raw material of following mass percent:
Thymol 0.1%, eugenol 0.1%, ethyl acetate 6%, EL-40 35%, dehydrated alcohol 4%, PEG400 1 %, distilled water 53.8%.
8. a compound recipe thymol Nano medication is characterized in that, is made up of the raw material of following mass percent:
Thymol 2%, eugenol 2%, ethyl acetate 1%, Tween-80 30%, dehydrated alcohol 5%, distilled water 60%.
9. the preparation method of the described compound recipe thymol of claim 1 Nano medication is characterized in that, specifically comprises the following steps:
1) take by weighing thymol, eugenol, oil phase, surfactant, cosurfactant, distilled water, standby;
2) thymol and eugenol are added in the oil phase, stir;
3) with step 2) solution of preparation adds to stir in the cosurfactant that it is dissolved fully, surfactant is added wherein again, stir;
4) solution with the step 3) preparation fully stirs at 20 ℃～25 ℃ slow down adding distilled water, has mobile yellow or water white compound recipe thymol Nano medication for a short time until formation clear, viscosity.
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| WO2017193221A1 (en) * | 2016-05-13 | 2017-11-16 | University Of Guelph | Compositions for controlled release of volatile compounds |
| CN108719457A (en) * | 2018-05-31 | 2018-11-02 | 武汉轻工大学 | Nanoemulsions and its preparation method and application with bacteriostatic activity thymol |
| CN108743950A (en) * | 2018-06-29 | 2018-11-06 | 佛山市南海东方澳龙制药有限公司 | Insecticide and preparation method thereof |
| CN112043817A (en) * | 2020-09-14 | 2020-12-08 | 北京皓尔生物科技有限公司 | Anti-mite composition and application thereof |
| CN115737611A (en) * | 2022-12-01 | 2023-03-07 | 成都科宏达科技有限公司 | Low-temperature stable animal medicated bath lotion |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105682669A (en) * | 2013-09-06 | 2016-06-15 | 马斯公司 | Oral anti-parasitic composition |
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| CN108719457A (en) * | 2018-05-31 | 2018-11-02 | 武汉轻工大学 | Nanoemulsions and its preparation method and application with bacteriostatic activity thymol |
| CN108743950A (en) * | 2018-06-29 | 2018-11-06 | 佛山市南海东方澳龙制药有限公司 | Insecticide and preparation method thereof |
| CN112043817A (en) * | 2020-09-14 | 2020-12-08 | 北京皓尔生物科技有限公司 | Anti-mite composition and application thereof |
| CN115737611A (en) * | 2022-12-01 | 2023-03-07 | 成都科宏达科技有限公司 | Low-temperature stable animal medicated bath lotion |
| CN115737611B (en) * | 2022-12-01 | 2024-05-14 | 成都科宏达科技有限公司 | Animal medicated bath lotion with low temperature stability |
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