CN103054733B - Chitosan nano-micelle wrappage solution and preparation method thereof - Google Patents
Chitosan nano-micelle wrappage solution and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a chitosan nano-micelle wrappage solution and a preparation method thereof. The preparation method of the chitosan nano-micelle wrappage solution is characterized by comprising the following steps of: 1. preparing a low-molecular-weight chitosan solution; 2. preparing a mixed liquid A from the low-molecular-weight chitosan solution and monounsaturated fatty acid; 3. carrying out nanofiltration on the mixed liquid A, so as to obtain a narrow-spectrum-molecular-weight chitosan solution; and 4. adding a surfactant into the narrow-spectrum-molecular-weight chitosan solution, and forming a nano-micelle by self-assembly, so as to obtain the chitosan nano-micelle wrappage solution. The chitosan nano-micelle wrappage solution disclosed by the invention is free of toxic and side effects to a human body, is also free of toxin, irritation and anaphylactic reaction and is safe and efficient, and the preparation method is simple, low in cost and high in profit and can be applied to the field of drugs or cosmetics.
Description
Technical field
The present invention relates to a kind of chitosan nano micelle wrappage solution and preparation method thereof.
Background technology
According to the < < of Ministry of Health of the People's Republic of China cosmetics health standard > >, define, cosmetics refer to embrocate, spray or other similar method, intersperse among any position of human body surface (skin, hair, fingernail, lip etc.), with the daily chemical industry product that reaches clean, eliminates bad smell, skin protection, beauty treatment and modification object.At present, the various dosage forms of all cosmetics, all mixture or chemistry and the biomaterial mixture of chemical material, even if they are made to nano-particle, and (nm cosmetic awaits further investigation to human skin cell's safety, subject matter is to prepare in material, whether to bring poisonous or allergin into, this will cause direct infringement to Skin Cell), its microscale harmful substance (as phthalic acid ester etc.) is to human body skin, hair, mucosa and enter and produce long term toxicity in body and injure by Transdermal absorption, even nano-particle plays irreversible effect to the DNA material of human body cell.
It to the research of nano medicament carrying system, is the new science that nanotechnology, biomaterial science are combined with Modern Pharmaceutics, to take nano grade biological macromolecular material as substrate, the new technique that medicine is combined with substrate in the mode of dissolving, absorption, parcel or bonding.The bioavailability that is applied as raising medicine and drug effect and the reduction poisonous side effect of medicine etc. of nano drug-carrying technology provide effective means.
Polymer drug slow-released carrier is divided into synthetic macromolecule (polylactic acid, polycaprolactone, polyacrylate etc.) and natural polymer (gelatin, cellulose, chitosan etc.).Synthetic macromolecule carrier usually biocompatibility is bad, sometimes also contains the toxic impurities such as trace initiator, can produce cytotoxicity.And natural polymer does not have above-mentioned shortcoming, wherein the research of chitosan receives much concern, this is because chitosan is naturally occurring unique alkaline polysaccharide, a kind of safety non-toxic, biodegradable natural polymer, not only there is biocompatibility, and there is the effects such as antibacterial, hemostasis, anticancer transfer.
Chitosan (chitosan) is the deacetylated product of chitin (chitin); there are good biocompatibility, biological degradability, reduced immunogenicity etc.; make it in biomedical materials field; as aspects such as medicine controlled releasing, organization brackets, bringing into play more and more important effect, causing and pay close attention to widely and study.In chitosan molecule structure, contain and be weakly alkaline free amine group, energy binding hydrogen ions, makes chitosan molecule surface band positive charge, therefore, chitosan is rendered as linear polymeric electrolyte under acid condition, and the solution of formation has certain viscosity, and this viscosity is directly proportional to its molecular mass.Meanwhile, in chitosan molecule structure, having a plurality of activity functional groups (comprising one-level and secondary hydroxyl, amide groups, amino and glycosidic bond etc.) can be for chemical modification so that the more derivant of preparation.Based on above-mentioned viewpoint, great many of experiments confirms that chitosan derivatives has multiple effect and purposes, expects that a series of macromolecular materials will play an important role at biomedicine field.Yet chitosan and chitosan derivatives are diverse two concepts: derivant is the compound being formed by connecting by covalent bond on chitosan basis, this is not natural product truly, therefore should it is exclusive in polysaccharide biomedicine.As pharmaceutical carrier, conventionally chitosan is prepared into its derivant, by the method hydrophobic synthetic side chain of chemistry or zymetology, this natural attribute to carrier itself is greatest provocation, and synthetic product must more or less exist the poisonous impurity such as trace or trace initiator.
In sum, nano medicament carrying system is carrying the developing direction of following pharmaceutics, is carrying people's expectation.And chitosan in natural polysaccharide material will played the part of more charming important role.The employing organic synthesis of abandoning tradition of the present invention or enzymatic synthesis chitosan block compound are prepared the method for nano drug-carrying material, take low-molecular weight chitoglycan as host material, by Electrostatic Absorption, ionomer and compound polyelectrolyte-surfactant self-assembling method, prepare water base chitosan nano micelle, wherein wrap up natural bacteriostatic and skin nutrition material, make chitosan nano micelle wrappage solution without any side effects.Yet, current relevant the method and pass through the chitosan nano micelle wrappage solution that the method makes and the research that is applied to cosmetic field have not been reported.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of and take natural low-molecular weight chitoglycan as host material, that by Electrostatic Absorption, ionomer and compound polyelectrolyte-surfactant self-assembling method, prepares makes chitosan nano micelle wrappage solution, and the preparation method of this chitosan nano micelle wrappage solution is provided.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A preparation method for chitosan nano micelle wrappage solution, is characterized in that, comprises the following steps:
The first step, prepares low-molecular weight chitoglycan solution by chitosan;
Second step adds monounsaturated fatty acid, then adds encapsulate substances in described low-molecular weight chitoglycan solution, obtains mixed liquor A after homogenizing;
The 3rd step, carries out nanofiltration processing to described mixed liquor A, obtains narrow spectrum molecular weight chitosan solution;
The 4th step adds surfactant in described narrow spectrum molecular weight chitosan solution, obtains chitosan nano micelle wrappage solution.
Further, described chitosan is selected the chitosan that deacetylation is 80%～90%, molecular weight is 80kDa～200kDa.
As a kind of embodiment, the first step, after chitosan is uniformly dissolved, adds hydrogenperoxide steam generator to prepare low-molecular weight chitoglycan solution.
Further, described hydrogenperoxide steam generator is 30% hydrogenperoxide steam generator.
Further, second step adds monounsaturated fatty acid in described low-molecular weight chitoglycan solution, add again encapsulate substances, and then be 20,000～50 by high pressure homogenizer or the rotating speed of 50～80Mpa, the high-shear homogenizer of 000rpm, obtains mixed liquor A after homogenizing.
Further again, described encapsulate substances is selected vitamin E, rose sandal savona quintessence oil or tea tree oil.
Further, the nanofiltration of described the 3rd step is processed and is comprised: described mixed liquor A is first carried out to nanofiltration infiltration NF 270-5040 rolled film and filter, remove the material below 4000 molecular weight, again filtrate is carried out to NF270-8040 rolled film and hold back 7000 following materials, leave and take nanofiltration liquid, obtain narrow spectrum molecular weight chitosan solution.
Further, the 4th step, described surfactant is selected the Tween-20 of 1.0%～40% narrow spectrum molecular weight chitosan solution weight, Tween-40, Tween-60, the PLURONICS F87 of a kind of or 1.0%～60% narrow spectrum molecular weight chitosan solution weight in Tween-80, a kind of in poloxamer188, or the Tween-20 of above-mentioned 1.0%～40% narrow spectrum molecular weight chitosan solution weight, Tween-40, Tween-60, the PLURONICS F87 of a kind of and above-mentioned 1.0%～60% narrow spectrum molecular weight chitosan solution weight in Tween-80, a kind of ratio by weight in poloxamer188 is 1～2: 1～3 mixture.
Further again, described the 4th step also comprises: the PEG-4000 or Polyethylene Glycol-1 that add 1.0%～40% narrow spectrum molecular weight chitosan solution weight, 000 or Polyethylene Glycol-7, 000, then high speed homogenization, by nanofiltration, process again, get water white transparency nanofiltration liquid, add the sodium lauroyl glutamate of 1%～15% narrow spectrum molecular weight chitosan solution weight or add the carbamide of 1%～10% narrow spectrum molecular weight chitosan solution weight and the sodium lauryl sulphate of 1%～10% narrow spectrum molecular weight chitosan solution weight, add again the pure water of 200%～400% narrow spectrum molecular weight chitosan solution weight to make chitosan nano micelle wrappage solution.
Further, the described high speed homogenization high-shear homogenizer homogenizing that to refer to by rotating speed be 20,000～50,000rpm.
Further, described nanofiltration is processed and is referred to by the nanofiltration of NF 270-9040 rolled film.
According to the preparation method of above-mentioned chitosan nano micelle wrappage solution, obtain chitosan nano micelle wrappage solution.
The invention has the beneficial effects as follows:
(1) ownership for material be safe, nontoxic, have no side effect, nonirritant, without the natural or chemical substance of allergenicity, the chitosan nano micelle wrappage solution composition that it prepares is simple, human body is had no side effect, safe, efficient, nontoxic, nonirritant, without anaphylaxis, be applied to medicine or cosmetic field, all suitable use of men and women, old and young.
(2) the present invention adopts ionomer method to prepare chitosan nano micelle, neither use any chemical substance or enzyme as initiator, also the extra high pressure homogenize dispersing emulsification machine that does not use expensive price, preparation method is simple, cost is low, and this has established good basis for the large production of scale;
(3) formation of chitosan nano micelle adopts self-assembling technique, removes a large amount of reagent and production equipment from, and production small investment, effective, and income is high;
(4) the present invention has overturned " compo " semar technique adopting in traditional lotion and cosmetics, but (human body the 6th vital principle) chitosan is wrapped up various to human body cell benefit materials as " peplos ", make minimum nanoparticle and bring into play maximum physiological effect, the great advantage of this challenge is that the nutrient substance of chitosan, human body cell physiological need is supplied with and maximized, and own intrinsic ultra trace toxin in various raw materials is minimized; Meanwhile, this method is also essentially different with the most modish " nm cosmetic ", is no longer the mixture that adds nanoparticle, but the aqueous solution of the Drug-loaded Nanoparticles;
(5) the present invention is can a side multiplex: adopt product prepared by manufacturing technique method of the present invention can make cosmetics and medicine for external use, can select to be prepared into different chitosan nano micelle wrappage solution according to different medicinal effects.For example, chitosan nano micelle parcel vitamin E solution is for cosmetics, can be to smear skin surface in order to beauty treatment, wrinkle resistant etc.; For medicine for external use, can be skin bacterio static itching-relieving varnish, medicine for rhinitis lotion, otitis media abluent, pudendum abluent, eye drops for cataract and degeneration of macula eye drop etc.
The specific embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein, only for description and interpretation the present invention, is not intended to limit the present invention.
Embodiment 1: the preparation of chitosan nano micelle parcel vitamin E solution
The preparation of step 1, low-molecular weight chitoglycan solution
Get respectively the raw material of following weight portion: deacetylation 80%, 1 part of 1 part of the chitosan of molecular weight 80kDa, 100 parts of pure water and acetic acid carry out stirring and dissolving at 50 ℃, and the solubilizing reaction time is 1h～24h.After being all uniformly dissolved to chitosan, add 30% hydrogenperoxide steam generator, the addition of 30% hydrogen peroxide is 2% of above-mentioned reactant gross weight, after stirring reaction 2h again, at 60 ℃ of vacuum concentration, to pasty state, until obtain water content, be 20% low-molecular weight chitoglycan solution.
The preparation of step 2, mixed liquor A
(1) preparation of high-purity monounsaturated fatty acid
Get respectively the raw material of following weight portion: 5 parts of fatty acid mixeds, 20 parts of methanol, 3 parts of polyglycerol esters, stirring reaction 2h, then at-50 ℃ of freezing 3h, sucking filtration, isolates satisfied fatty acid and filtrate, reclaims methanol obtain unsaturated fatty acid from filtrate; The unsaturated fatty acid that is 5:1 by parts by weight ratio again and magnetic Nano argentum powder stirring reaction 24h(magnetic Nano argentum powder π complexation absorption polyunsaturated fatty acid), with the separated nanometer silver in stationary magnetic field, separatory takes out water white transparency fluid and carries out molecular distillation, obtains high-purity (95%) monounsaturated fatty acid.
(2) above-mentioned high-purity (95% oleic acid) monounsaturated fatty acid that adds 6% low-molecular weight chitoglycan solution weight in the low-molecular weight chitoglycan solution preparing in step 1, drip again the vitamin E with monounsaturated fatty acid equivalent, by high pressure homogenizer 50MPa homogenizing twice, obtain mixed liquor A (chitosan monounsaturated fatty acid (95% oleic acid) salt parcel and/or the absorption microemulsion of vitamin E and the mixed liquor of emulsion).
Step 3, hold back narrow spectrum molecular weight chitosan
Mixed liquor A after step 2 homogenizing is carried out to nanofiltration infiltration NF 270-5040 rolled film and filter, remove the material below 4,000 molecular weight, again filtrate is carried out to NF 270-8040 rolled film and hold back 7,000 following material, leaves and takes nanofiltration liquid, obtains narrow spectrum molecular weight chitosan solution.
The formation of step 4, narrow spectrum molecular weight chitosan solution and surfactant self-assembled nano micelle
In narrow spectrum molecular weight chitosan solution, the mixture that adds the Tween-20 of 1.0% narrow spectrum molecular weight chitosan solution weight and the PLURONICS F87 of 1.0% narrow spectrum molecular weight chitosan solution weight, the PEG-4000 that adds again 1.0% narrow spectrum molecular weight chitosan solution weight, high speed homogenization rotating speed is 20, 000rpm, and then by nanofiltration NF 270-9040 rolled film, get water white transparency nanofiltration liquid, the sodium lauroyl glutamate that adds 1.0% narrow spectrum molecular weight chitosan solution weight, finally add the pure water of 200% narrow spectrum molecular weight chitosan solution weight to make chitosan nano micelle parcel vitamin E aqueous solution.
Embodiment 2: the preparation of chitosan nano micelle parcel vitamin E solution
The preparation of step 1, low-molecular weight chitoglycan solution
Get respectively the raw material of following weight portion: deacetylation 85%, 1 part of 2 parts of the chitosans of molecular weight 140kDa, 150 parts of pure water and acetic acid, carry out stirring and dissolving at 60 ℃, and the solubilizing reaction time is 1h～24h.After being all uniformly dissolved, add 30% hydrogenperoxide steam generator, the addition of 30% hydrogen peroxide is 6% of above-mentioned reactant gross weight, stirring reaction 6h, whole at 70 ℃ of vacuum concentration to pasty state, until obtain water content, be 40% low-molecular weight chitoglycan solution.
The preparation of step 2, mixed liquor A
(1) preparation of high-purity monounsaturated fatty acid
Get respectively the raw material of following weight portion: 6 parts of 7 parts of fatty acid mixeds, 50 parts of methanol and polyglycerol esters, stirring reaction 6h, at-40 ℃ of freezing 13h, sucking filtration, isolates satisfied fatty acid and filtrate, and filtrate is reclaimed methanol and is obtained unsaturated fatty acid; The unsaturated fatty acid that is 7: 2 by parts by weight ratio again and magnetic Nano argentum powder (magnetic Nano argentum powder π complexation absorption polyunsaturated fatty acid) stirring reaction 48h, with the separated nanometer silver in stationary magnetic field, separatory takes out water white transparency fluid and carries out molecular distillation, obtains high-purity (90%) monounsaturated fatty acid.
(2) above-mentioned high-purity (90%) monounsaturated fatty acid that adds 10% low-molecular weight chitoglycan solution weight in the low-molecular weight chitoglycan solution preparing in step 1, drip again the vitamin E with monounsaturated fatty acid equivalent, high pressure homogenizer 70MPa homogenizing twice, obtains mixed liquor A (chitosan monounsaturated fatty acid (90% oleic acid) salt parcel and/or the absorption microemulsion of vitamin E and the mixed liquor of emulsion).
Step 3, hold back narrow spectrum molecular weight chitosan
Mixed liquor A after step 2 homogenizing is carried out to nanofiltration infiltration NF 270-5040 rolled film and filter, remove the material below 4,000 molecular weight, again filtrate is carried out to NF 270-8040 rolled film and hold back 7,000 following material, leaves and takes nanofiltration liquid, obtains narrow spectrum molecular weight chitosan solution.
The formation of step 4, narrow spectrum molecular weight chitosan solution and surfactant self-assembled nano micelle
In narrow spectrum molecular weight chitosan solution, the Tween-40 that adds 10% narrow spectrum molecular weight chitosan solution weight, the PEG-6000 of 10% narrow spectrum molecular weight chitosan solution, high speed homogenization rotating speed is 40, 000rpm, and then by nanofiltration NF 270-9040 rolled film, get water white transparency nanofiltration liquid, the carbamide that adds 1% narrow spectrum molecular weight chitosan solution weight, the sodium lauryl sulphate of 1% narrow spectrum molecular weight chitosan solution weight, the pure water of the sodium lauroyl glutamate of 15% narrow spectrum molecular weight chitosan solution weight and 300% narrow spectrum molecular weight chitosan solution weight is made chitosan nano micelle parcel vitamin E aqueous solution.
Embodiment 3: the preparation of chitosan nano micelle parcel vitamin E solution
The preparation of step 1, low-molecular weight chitoglycan solution
Get respectively the raw material of following weight portion: deacetylation 90%, 2 parts of 3 parts of the chitosans of molecular weight 200kDa, 200 parts of pure water and acetic acid, carry out stirring and dissolving at 70 ℃, and the solubilizing reaction time is 1h～24h.After being all uniformly dissolved, add 30% hydrogenperoxide steam generator, the addition of 30% hydrogen peroxide is 10% of above-mentioned reactant gross weight, stirring reaction 10h, whole at 80 ℃ of vacuum concentration to pasty state, until obtain water content, be 60% low-molecular weight chitoglycan solution.
The preparation of step 2, mixed liquor A
(1) selection of fatty acid: directly select chemical pure monounsaturated fatty acid, for example 60% oleic acid.
(2) the above-mentioned monounsaturated fatty acid (60% oleic acid) that adds 15% low-molecular weight chitoglycan solution weight in the low-molecular weight chitoglycan solution preparing in step 1, drip again the vitamin E with monounsaturated fatty acid equivalent, high pressure homogenizer 80MPa homogenizing twice, obtains mixed liquor A (chitosan monounsaturated fatty acid (60% oleic acid) salt parcel and/or the absorption microemulsion of vitamin E and the mixed liquor of emulsion).
Step 3, hold back narrow spectrum molecular weight chitosan
Mixed liquor A after step 2 homogenizing is carried out to nanofiltration infiltration NF 270-5040 rolled film and filter, remove the material below 4,000 molecular weight, again filtrate is carried out to NF 270-8040 rolled film and hold back 7,000 following material, leaves and takes nanofiltration liquid, obtains narrow spectrum molecular weight chitosan solution.
The formation of step 4, narrow spectrum molecular weight chitosan solution and surfactant self-assembled nano micelle
In narrow spectrum molecular weight chitosan solution, add the Tween-80 of 40% narrow spectrum molecular weight chitosan solution weight and the poloxamer188 mixture of 60% narrow spectrum molecular weight chitosan solution weight, Polyethylene Glycol-7 that add again 40% narrow spectrum molecular weight chitosan solution weight, 000, high speed homogenization rotating speed is 50, 000rpm, and then by nanofiltration NF 270-9040 rolled film, get water white transparency nanofiltration liquid, the carbamide that adds 10% narrow spectrum molecular weight chitosan solution weight, the pure water of the sodium lauryl sulphate of 10% narrow spectrum molecular weight chitosan solution weight and 400% narrow spectrum molecular weight chitosan solution weight is made chitosan nano micelle parcel vitamin E aqueous solution.
Embodiment 4: the preparation of chitosan nano micelle parcel rose sandal savona quintessence oil solution
The preparation of step 1, low-molecular weight chitoglycan solution
Get respectively the raw material of following weight portion: deacetylation 80%, 1 part of 1 part of the chitosan of molecular weight 80kDa, 100 parts of pure water and acetic acid carry out stirring and dissolving at 50 ℃, and the solubilizing reaction time is 1h～24h.After being all uniformly dissolved to chitosan, add 30% hydrogenperoxide steam generator, the addition of 30% hydrogen peroxide is 2% of above-mentioned reactant gross weight, after stirring reaction 2h again, at 60 ℃ of vacuum concentration, to pasty state, until obtain water content, be 20% low-molecular weight chitoglycan solution.
The preparation of step 2, mixed liquor A
(1) preparation of high-purity monounsaturated fatty acid
Get respectively the raw material of following weight portion: 5 parts of fatty acid mixeds, 20 parts of methanol, 3 parts of polyglycerol esters, stirring reaction 2h, then at-50 ℃ of freezing 3h, sucking filtration, isolates satisfied fatty acid and filtrate, and filtrate is reclaimed methanol and is obtained unsaturated fatty acid; The unsaturated fatty acid that is 5:1 by parts by weight ratio again and magnetic Nano argentum powder (magnetic Nano argentum powder π complexation absorption polyunsaturated fatty acid) stirring reaction 24h, with the separated nanometer silver in stationary magnetic field, separatory takes out water white transparency fluid and carries out molecular distillation, obtains high-purity (95%) monounsaturated fatty acid.
(2) above-mentioned high-purity (95%) monounsaturated fatty acid that adds 6% low-molecular weight chitoglycan solution weight in the low-molecular weight chitoglycan solution preparing in step 1, drip again the rose sandal savona quintessence oil with monounsaturated fatty acid equivalent, by high pressure homogenizer 50MPa homogenizing twice, obtain mixed liquor A (microemulsion of chitosan monounsaturated fatty acid (95% oleic acid) salt parcel and/or absorption rose sandal savona quintessence oil and the mixed liquor of emulsion).
Step 3, hold back narrow spectrum molecular weight chitosan
Mixed liquor A after step 2 homogenizing is carried out to nanofiltration infiltration NF 270-5040 rolled film and filter, remove the material below 4,000 molecular weight, again filtrate is carried out to NF 270-8040 rolled film and hold back 7,000 following material, leaves and takes nanofiltration liquid, obtains narrow spectrum molecular weight chitosan solution.
The formation of step 4, narrow spectrum molecular weight chitosan solution and surfactant self-assembled nano micelle
In narrow spectrum molecular weight chitosan solution, the mixture that adds the Tween-20 of 1.0% narrow spectrum molecular weight chitosan solution weight and the PLURONICS F87 of 1.0% narrow spectrum molecular weight chitosan solution weight, the PEG-4000 that adds again 1.0% narrow spectrum molecular weight chitosan solution weight, high speed homogenization rotating speed is 20, 000rpm, and then by nanofiltration NF 270-9040 rolled film, get water white transparency nanofiltration liquid, the sodium lauroyl glutamate that adds 1% narrow spectrum molecular weight chitosan solution weight, finally add the pure water of 200% narrow spectrum molecular weight chitosan solution weight to make chitosan nano micelle parcel rose sandal savona quintessence oil aqueous solution.
Embodiment 5: the preparation of chitosan nano micelle parcel tea tree oil solution
The preparation of step 1, low-molecular weight chitoglycan solution
Get respectively the raw material of following weight portion: deacetylation 90%, 2 parts of 3 parts of the chitosans of molecular weight 200kDa, 200 parts of pure water and acetic acid, carry out stirring and dissolving at 70 ℃, and the solubilizing reaction time is 1h～24h.After being all uniformly dissolved, add 30% hydrogenperoxide steam generator, the addition of 30% hydrogen peroxide is 10% of above-mentioned reactant gross weight, stirring reaction 10h, whole at 80 ℃ of vacuum concentration to pasty state, until obtain water content, be 60% low-molecular weight chitoglycan solution.
The preparation of step 2, mixed liquor A
(1) selection of fatty acid: directly select chemical pure monounsaturated fatty acid, for example 60% oleic acid.
(2) the above-mentioned monounsaturated fatty acid (60% oleic acid) that adds 15% low-molecular weight chitoglycan solution weight in the low-molecular weight chitoglycan solution preparing in step 1, drip again the tea tree oil with monounsaturated fatty acid equivalent, high pressure homogenizer 80MPa homogenizing twice, obtains mixed liquor A (chitosan monounsaturated fatty acid (60% oleic acid) salt parcel and/or the absorption microemulsion of tea tree oil and the mixed liquor of emulsion).
Step 3, hold back narrow spectrum molecular weight chitosan
Mixed liquor A after step 2 homogenizing is carried out to nanofiltration infiltration NF 270-5040 rolled film and filter, remove the material below 4,000 molecular weight, again filtrate is carried out to NF 270-8040 rolled film and hold back 7,000 following material, leaves and takes nanofiltration liquid, obtains narrow spectrum molecular weight chitosan solution.
The formation of step 4, narrow spectrum molecular weight chitosan solution and surfactant self-assembled nano micelle
In narrow spectrum molecular weight chitosan solution, add the Tween-80 of 40% narrow spectrum molecular weight chitosan solution weight and the poloxamer188 mixture of 60% narrow spectrum molecular weight chitosan solution weight, Polyethylene Glycol-7 that add again 40% narrow spectrum molecular weight chitosan solution weight, 000, high speed homogenization rotating speed is 50, 000rpm, and then by nanofiltration NF 270-9040 rolled film, get water white transparency nanofiltration liquid, the carbamide that adds 5% narrow spectrum molecular weight chitosan solution weight, the pure water of the sodium lauryl sulphate of 5% narrow spectrum molecular weight chitosan solution weight and 400% narrow spectrum molecular weight chitosan solution weight is made chitosan nano micelle parcel tea tree oil aqueous solution.
In the above-described embodiments; fatty acid mixed, methanol, polyglycerol ester, oleic acid, vitamin E, Tween-20, Tween-40, Tween-60, Tween-80, PLURONICS F87, poloxamer188, PEG-4000 or Polyethylene Glycol-1; 000 or Polyethylene Glycol-7; 000, sodium lauroyl glutamate, carbamide, sodium lauryl sulphate etc. are all selected commercially available prod, the fatty acid mixed that wherein fatty acid mixed preferred oil acid content is 50%～70%.
The above-mentioned chitosan nano micelle wrappage aqueous solution preparing is tested:
1, the bacteriostatic test of chitosan nano micelle wrappage aqueous solution (GB 15979-2002)
Select the chitosan nano micelle wrappage aqueous solution of above-described embodiment 1～5 to do bacteriostatic test, result is as follows:
2, the histamine of chitosan nano micelle wrappage aqueous solution causes the resistance test of itching
Select the chitosan nano micelle wrappage aqueous solution of above-described embodiment 1～5 to do histamine and cause the resistance test of itching, result is as follows:
| Experiment group | Histamine itch-threshold value (μ gL -1) |
| Blank | 32.2±16.5 |
| PIYANPING contrast | 329.2±48.7 |
| Embodiment 1 sample | 337.5±28.7 |
| Embodiment 2 samples | 322.1±31.4 |
| Embodiment 3 samples | 281.7±36.3 |
| Embodiment 4 samples | 378.9±22.3 |
| Embodiment 5 samples | 389.3±18.7 |
Finally it should be noted that: these are only the preferred embodiments of the present invention; be not limited to the present invention; although the present invention is had been described in detail with reference to embodiment; for a person skilled in the art; its technical scheme that still can record aforementioned each embodiment is modified; or part technical characterictic is wherein equal to replacement; but within the spirit and principles in the present invention all; any modification of doing, be equal to replacement, improvement etc., within protection scope of the present invention all should be included in.
Claims (8)
1. a preparation method for chitosan nano micelle wrappage solution, is characterized in that, comprises the following steps:
The first step, after chitosan is uniformly dissolved, adds hydrogenperoxide steam generator to prepare low-molecular weight chitoglycan solution;
Second step adds monounsaturated fatty acid, then adds encapsulate substances in described low-molecular weight chitoglycan solution, obtains mixed liquor A after homogenizing;
The 3rd step, described mixed liquor A is carried out to nanofiltration processing, obtain narrow spectrum molecular weight chitosan solution, described nanofiltration is processed and is comprised: described mixed liquor A is first carried out to nanofiltration infiltration NF270-5040 rolled film and filter, remove the material below 4000 molecular weight, again filtrate is carried out to NF270-8040 rolled film and hold back 7000 following materials, leave and take nanofiltration liquid, obtain narrow spectrum molecular weight chitosan solution;
The 4th step adds surfactant in described narrow spectrum molecular weight chitosan solution, obtains chitosan nano micelle wrappage solution, described surfactant is selected the Tween-20 of 1.0%～40% narrow spectrum molecular weight chitosan solution weight, Tween-40, Tween-60, the PLURONICS F87 of a kind of or 1.0%～60% narrow spectrum molecular weight chitosan solution weight in Tween-80, a kind of in poloxamer188, or the Tween-20 of above-mentioned 1.0%～40% narrow spectrum molecular weight chitosan solution weight, Tween-40, Tween-60, the PLURONICS F87 of a kind of and above-mentioned 1.0%～60% narrow spectrum molecular weight chitosan solution weight in Tween-80, a kind of ratio by weight in poloxamer188 is 1～2: 1～3 mixture, described the 4th step also comprises: the PEG-4000 or Polyethylene Glycol-1 that add 1.0%～40% narrow spectrum molecular weight chitosan solution weight, 000 or Polyethylene Glycol-7, 000, then high speed homogenization, by nanofiltration, process again, get water white transparency nanofiltration liquid, add the sodium lauroyl glutamate of 1%～15% narrow spectrum molecular weight chitosan solution weight or add the carbamide of 1%～10% narrow spectrum molecular weight chitosan solution weight and the sodium lauryl sulphate of 1%～10% narrow spectrum molecular weight chitosan solution weight, add again the pure water of 200%～400% narrow spectrum molecular weight chitosan solution weight to make chitosan nano micelle wrappage solution.
2. the preparation method of chitosan nano micelle wrappage solution according to claim 1, is characterized in that, described chitosan is selected the chitosan that deacetylation is 80%～90%, molecular weight is 80kDa～200kDa.
3. the preparation method of chitosan nano micelle wrappage solution according to claim 1, is characterized in that, described hydrogenperoxide steam generator is 30% hydrogenperoxide steam generator.
4. the preparation method of chitosan nano micelle wrappage solution according to claim 1, it is characterized in that, second step, in described low-molecular weight chitoglycan solution, add monounsaturated fatty acid, add again encapsulate substances, and then be 20,000～50 by high pressure homogenizer or the rotating speed of 50～80Mpa, the high-shear homogenizer of 000rpm, obtains mixed liquor A after homogenizing.
5. the preparation method of chitosan nano micelle wrappage solution according to claim 1, is characterized in that, described encapsulate substances is selected vitamin E, rose sandal savona quintessence oil or tea tree oil.
6. the preparation method of chitosan nano micelle wrappage solution according to claim 1, is characterized in that, the high-shear homogenizer homogenizing that it is 20,000～50,000rpm that described high speed homogenization refers to by rotating speed.
7. the preparation method of chitosan nano micelle wrappage solution according to claim 1, is characterized in that, the nanofiltration of described the 4th step is processed and referred to by the nanofiltration of NF270-9040 rolled film.
8. the chitosan nano micelle wrappage solution obtaining according to the preparation method of the arbitrary described chitosan nano micelle wrappage solution of claim 1-7.
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