CN107550860A - A kind of acetylisovaleryl tylosin nano-emulsion and preparation method thereof - Google Patents
A kind of acetylisovaleryl tylosin nano-emulsion and preparation method thereof Download PDFInfo
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- CN107550860A CN107550860A CN201710830132.0A CN201710830132A CN107550860A CN 107550860 A CN107550860 A CN 107550860A CN 201710830132 A CN201710830132 A CN 201710830132A CN 107550860 A CN107550860 A CN 107550860A
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- acetylisovaleryl tylosin
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Abstract
The invention discloses a kind of acetylisovaleryl tylosin nano-emulsion and preparation method thereof, represented with parts by weight, mainly by 30 ~ 50 parts of Tween 80s, 5 ~ 20 parts of absolute ethyl alcohols, 1 ~ 10 part of ethyl acetate, 1 ~ 5 part of acetylisovaleryl tylosin, enough distilled water compositions.Nano-emulsion caused by the present invention is oil-in-water type nano-emulsion, can use water infinite dilution.Under transmission electron microscope, nano-emulsion is rounded, and nothing is adhered.Average grain diameter（Z‑Average）For 12.3nm, polydispersity coefficient（PDI）For 0.207.At 25 DEG C, the average zeta current potentials of the Angelica grosseserrata volatile oil nano-emulsion after 5 times of dilution are（‑11.4±0.3）MV, it has good stability with thermostatic accelerated experiment result collectively show that；The nano-emulsion preparation technology is simple and quality controllable, and antiphlogistic effects are good, is expected to be applied to clinic.
Description
Technical field
The present invention relates to nano-emulsion preparation field, in particular to a kind of acetylisovaleryl tylosin nano-emulsion and its preparation
Method.
Background technology
Nanoemulsions（nanoemulsion）Also known as microemulsion（microemulsion）, it is by water, oil, EL-40 and 1,2-
Propane diols etc. spontaneously forms, and particle diameter is 1~100nm Thermodynamically stable, isotropism, transparent or semitransparent homogeneous dispersion
Be in general, nano-emulsion is divided into three types, i.e. oil-in-water type nano-emulsion (O/W), water-in-oil type nanoemulsion (W/O and double
Continuous type nano-emulsion (B.C), nineteen forty-three are found and report this dispersion first by Hoar and Schulman.Until 1959
Year, Schulman just proposes " microemulsion " this concept.Hereafter, the theory of nano-emulsion and application study obtain fast
The development of speed.At present, nanometer emulsified technology has penetrated into daily-use chemical industry, fine chemistry industry, petrochemical industry, material science, biological skill
The field such as art and environmental science, turn into the current research field in the world with huge applications potentiality.
Nano-emulsion has the advantages of many other preparations are incomparable：1. being isotropic transparency liquid, belong to thermodynamics
Systems stabilisation, it can not be allowed to be layered through pressure sterilizing or centrifugation；2. technique is simple, preparation process is not required to special installation, can be certainly
Hair is formed, and nano-emulsion particle diameter is generally 1~100nm；3. viscosity is low, pain during injection can be reduced；4. with sustained release and targeting
Effect；5. improving the solubility of medicine, the enzymolysis of medicine in vivo is reduced, the protective effect to medicine can be formed and improve stomach and intestine
Absorption of the road to medicine, improve the bioavilability of medicine.Therefore nano-emulsion is widely paid close attention to as a kind of pharmaceutical carrier.
Acetylisovaleryl tylosin（Acetylisovaleryltylosin, it is abbreviated as AIV）It is that a kind of new Thailand is happy
Streptozotocin derivative, AIV have a good antibacterial activity, and clinic is mainly used in treating the acute and chronic breathing problem of poultry, pig
The diseases such as the red dysentery of asthma, pig, mycoplasmal arthritis.But the solubility of acetylisovaleryl tylosin and stability are
Shortcoming, in terms of clinical application is carried out, by very big restriction.
The content of the invention
It is an object of the invention to provide a kind of effective acetyl isoamyl for improving acetylisovaleryl tylosin stability
Acyl tylosin nano-emulsion.
It is another object of the present invention to provide the preparation method of above-mentioned acetylisovaleryl tylosin nano-emulsion.
The present invention is achieved through the following technical solutions：A kind of acetylisovaleryl tylosin nano-emulsion, is represented with parts by weight,
Mainly by 30 ~ 50 parts of Tween-80s, 5 ~ 20 parts of absolute ethyl alcohols, 1 ~ 10 part of ethyl acetate, 1 ~ 5 part of acetylisovaleryl tylosin, foot
Measure distilled water composition.
In order to which the present invention is better achieved, further, represented with parts by weight, the Tween-80 is 25 parts, absolute ethyl alcohol
Be 4.4 parts for 15 parts, ethyl acetate, acetylisovaleryl tylosin be 1 part, and distilled water be 54.6 parts.
A kind of preparation method of above-mentioned acetylisovaleryl tylosin nano-emulsion, comprises the following steps：
（1）Tween-80 is added in four-hole boiling flask, acetylisovaleryl tylosin, ethyl acetate, stirring makes it well mixed；
（2）Four-hole boiling flask is fixed under water bath condition, water temperature is maintained at 40 ~ 60 DEG C, after raw material fully melts, starts stirring
Device, mixing speed are 150 ~ 200rpm；
（3）After material temperature in four-hole boiling flask up to after 40 ~ 60 DEG C, stop stirring, add absolute ethyl alcohol, continue to stir, continue
30min；
（4）Stop stirring, 40 ~ 60 DEG C of hot distilled waters are added dropwise with rubber head dropper, after 3 ~ 8h is added dropwise to complete, 1h is incubated in 40 ~ 60 DEG C；
（5）Heating water bath is closed, after being cooled to normal temperature, adds bactericide, continues to stir 30min；
（6）After 5 ~ 10 DEG C being cooled to using cold bath, filtering and discharging.
In order to which the preparation of nano-emulsion in the present invention is better achieved, further, the stirring used in the preparation process
Device is magnetic stirring apparatus.
In order to which the preparation of nano-emulsion in the present invention is better achieved, further, the step（4）In, thermal distillation is added dropwise
Water uses rubber head dropper.
In order to which the preparation of nano-emulsion in the present invention is better achieved, further, the step（4）In, thermal distillation is added dropwise
The process of water is that a drop is added dropwise in every 3 ~ 4min, per 2 ~ 3ml of dropper.
The present invention compared with prior art, has advantages below and beneficial effect：
（1）Nano-emulsion caused by the present invention is oil-in-water type nano-emulsion, can use water infinite dilution.Under transmission electron microscope, nano-emulsion is in circle
Spherical, nothing is adhered.Average grain diameter（Z-Average）For 12.3nm, polydispersity coefficient（PDI）For 0.207.At 25 DEG C, dilution 5
The average zeta current potentials of Angelica grosseserrata volatile oil nano-emulsion after times are（-11.4±0.3）MV, with the common table of thermostatic accelerated experiment result
Bright its has good stability；
（2）Nano-emulsion preparation technology of the present invention is simple and quality controllable, and antiphlogistic effects are good, is expected to be applied to clinic.
Embodiment
The present invention is described in further detail with reference to embodiment, but the implementation of the present invention is not limited to this,
Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, various replace is made
Change and change, all should be included within the scope of the invention.
Embodiment：
The acetylisovaleryl tylosin nano-emulsion of the present embodiment, as mass fraction：w（Acetylisovaleryl tylosin）=1%,
w（Ethyl acetate）=4.4%, w（Absolute ethyl alcohol）=15%, w（Tween-80）=25%, w（Distilled water）=54.6%.
Its preparation method, comprise the following steps：
（1）EL-40 is added in four-hole boiling flask, acetylisovaleryl tylosin, EL-40, RH-40, stirring makes it well mixed；
（2）Four-hole boiling flask is fixed under water bath condition, water temperature is maintained at 40 ~ 60 DEG C, after raw material fully melts, starts stirring
Device, mixing speed are 150 ~ 200rpm；
（3）After material temperature in four-hole boiling flask up to after 40 ~ 60 DEG C, stop stirring, add PEG-400, continue to stir, continue
30min；
（4）Stop stirring, 40 ~ 60 DEG C of hot distilled waters are added dropwise with rubber head dropper, after 3 ~ 8h is added dropwise to complete, 1h is incubated in 40 ~ 60 DEG C；
（5）Heating water bath is closed, after being cooled to normal temperature, adds bactericide, continues to stir 30min；
（6）After 5 ~ 10 DEG C being cooled to using cold bath, filtering and discharging.
According to solubility and pseudo-ternary phase diagram of the AIV in oil phase and cosurfactant, to oil phase, surfactant,
Cosurfactant, K m values are screened；With decoration method, differentiate nano-emulsion structure type；With transmission electron microscope and grain size analysis
Instrument, investigate AIV-NE form and particle diameter distribution；It is stable that it is investigated by high speed centrifugation, accelerated test and long term test
Property；Establish the ultraviolet spectrophotometry of AIV assays in AIV-NE；Investigate AIV-NE's by acute toxicity test in mice
Security；Antibacterial activities of the AIV-NE to 5 kinds of encountered pathogenic bacterias is evaluated by extracorporeal bacteria inhibitor test；Healthy chick is attacked
Poison, it is infected staphylococcus aureus, animal is divided into the high, medium and low dosage groups of AIV-NE, AIV bulk drugs control group, for rice
Star solution control group, infection control group and healthy control group are examined, investigates treated effect and healing of each administration group to ill chicken
Rate, drug effect inside nano-emulsion is evaluated.
The ultraviolet spectrophotometry of the foundation specificity is good, and the rate of recovery, repeatability and precision meet the requirements.AIV-
NE median lethal dose（LD 50 ）For 2425 mg/kg, the 95% of LD 50 credible is limited to：2204~2707 mg/kg, belong to
Low toxicity level medicine.AIV-NE to Escherichia coli, staphylococcus aureus, salmonella, Pasteurella and Streptococcusagalactiae most
Small Mlc（MIC）Respectively 16,2,8,4,8 μ g/mL, respectively less than AIV solution and tilmicosin solution group, and difference pole
Significantly（P<0.01）.The cure rate of the high, medium and low dosage groups of AIV-NE is respectively 96.7%, 93.3%, 76.7%, and effective percentage is respectively
100%、96.7%、83.3%；The cure rate of AIV bulk drug control groups is 66.7%, and effective percentage is 76.7%；Tilmicosin solution pair
Cure rate according to group is 60%, and effective percentage is 66.7%.Analyzed by statistic law, AIV-NE height, the significant figure of middle dose group, healing
Number and weightening are significantly better than AIV solution group and tilmicosin solution group.
Embodiment 2：
It is equal further to limit the agitator used in the preparation process in order to preferably realize the preparation of nano-emulsion for the present embodiment
For magnetic stirring apparatus.The present embodiment other parts are same as the previously described embodiments, repeat no more here.
Embodiment 3：
The present embodiment further limits the step to preferably realize the preparation of nano-emulsion（4）In, hot distilled water, which is added dropwise, to be made
It is rubber head dropper.The present embodiment other parts are same as the previously described embodiments, repeat no more here.
Embodiment 4；
The present embodiment further limits the step to preferably realize the preparation of nano-emulsion（4）In, hot distilled water is added dropwise
Process is that a drop is added dropwise in every 3 ~ 4min, per 2 ~ 3ml of dropper.The present embodiment other parts are same as the previously described embodiments, here no longer
Repeat.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that：Not
A variety of change, modification, replacement and modification can be carried out to these embodiments by departing under the principle and objective of the present invention, of the invention
Scope is limited by claim and its equivalent.
Claims (6)
- A kind of 1. acetylisovaleryl tylosin nano-emulsion, it is characterised in that：Represented with parts by weight, mainly by 30 ~ 50 parts of tweens- 80th, 5 ~ 20 parts of absolute ethyl alcohols, 1 ~ 10 part of ethyl acetate, 1 ~ 5 part of acetylisovaleryl tylosin, enough distilled water compositions.
- A kind of 2. acetylisovaleryl tylosin nano-emulsion according to claim 1, it is characterised in that：With parts by weight table Showing, the Tween-80 is 25 parts, absolute ethyl alcohol is 15 parts, ethyl acetate is 4.4 parts, acetylisovaleryl tylosin is 1 part, And distilled water is 54.6 parts.
- A kind of 3. preparation method of acetylisovaleryl tylosin nano-emulsion according to claim 1 or claim 2, it is characterised in that Comprise the following steps：（1）Tween-80 is added in four-hole boiling flask, acetylisovaleryl tylosin, ethyl acetate, stirring makes it well mixed；（2）Four-hole boiling flask is fixed under water bath condition, water temperature is maintained at 40 ~ 60 DEG C, after raw material fully melts, starts stirring Device, mixing speed are 150 ~ 200rpm；（3）After material temperature in four-hole boiling flask up to after 40 ~ 60 DEG C, stop stirring, add absolute ethyl alcohol, continue to stir, continue 30min；（4）Stop stirring, 40 ~ 60 DEG C of hot distilled waters are added dropwise with rubber head dropper, after 3 ~ 8h is added dropwise to complete, 1h is incubated in 40 ~ 60 DEG C；（5）Heating water bath is closed, after being cooled to normal temperature, adds bactericide, continues to stir 30min；（6）After 5 ~ 10 DEG C being cooled to using cold bath, filtering and discharging.
- A kind of 4. acetylisovaleryl tylosin nano-emulsion according to claim 3, it is characterised in that：The preparation process The middle agitator used is magnetic stirring apparatus.
- A kind of 5. acetylisovaleryl tylosin nano-emulsion according to claim 3 or 4, it is characterised in that：The step （4）In, hot distilled water is added dropwise and uses rubber head dropper.
- A kind of 6. acetylisovaleryl tylosin nano-emulsion according to claim 5, it is characterised in that：The step（4） In, a drop is added dropwise for every 3 ~ 4min in the process that hot distilled water is added dropwise, per 2 ~ 3ml of dropper.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109820822A (en) * | 2019-03-21 | 2019-05-31 | 天津市保灵动物保健品有限公司 | A kind of compound tylosin microemulsion injection and its preparation method and application containing sulfa drugs |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274178A (en) * | 2011-08-25 | 2011-12-14 | 西北农林科技大学 | Acetyl-isovaleryl tylosin nanoemulsion medicine and preparation method thereof |
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- 2017-09-15 CN CN201710830132.0A patent/CN107550860A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274178A (en) * | 2011-08-25 | 2011-12-14 | 西北农林科技大学 | Acetyl-isovaleryl tylosin nanoemulsion medicine and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109820822A (en) * | 2019-03-21 | 2019-05-31 | 天津市保灵动物保健品有限公司 | A kind of compound tylosin microemulsion injection and its preparation method and application containing sulfa drugs |
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