CN103156784B - Chitosan-fullerol compound, preparation method thereof compound and moisture-preserving antioxidant - Google Patents
Chitosan-fullerol compound, preparation method thereof compound and moisture-preserving antioxidant Download PDFInfo
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- CN103156784B CN103156784B CN201310100766.2A CN201310100766A CN103156784B CN 103156784 B CN103156784 B CN 103156784B CN 201310100766 A CN201310100766 A CN 201310100766A CN 103156784 B CN103156784 B CN 103156784B
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Abstract
The invention discloses a chitosan-fullerol compound, a preparation method thereof and a moisture-preserving antioxidant. The preparation method comprises the steps of: counting in mass ratio, dissolving 98-99.5% of water soluble chitosan and 0.5-2% of fullerol into a mixed solvent, and preparing spinning solution by adequately stirring; carrying out electrospinning on the uniformly stirred spinning solution; and dissolving non-woven fabrics obtained by the electrospinning into water, so as to obtain the chitosan-fullerol compound. According to the preparation method, by carrying out electrospinning on mixed solution of the chitosan and the fullerol, the chitosan-fullerol compound is prepared and obtained from the obtained non-woven fabrics; and by carrying out proper derivatization on the fullerol, not only can the excellent physiological activity of the fullerol be continued, but also the negative factors caused by a relatively large amount of hydroxyl groups are decreased, so that the application range and field of the fullerol are expanded.
Description
Technical field
The present invention relates to richness and strangle alcohol composite materials field, relate in particular to a kind of chitosan-Fu Le alcohol complex, its preparation method, moisturizing antioxidant.
Background technology
Richness is strangled alcohol (C
60(OH)
n) as research a kind of water-soluble fullerenes derivates comparatively widely, show excellent performance at biomedical sector.But strangling alcohol itself due to richness is to rely on that Fullerene Carbon cage is outer modifies upper water soluble group-hydroxyl, reach and improve biocompatibility, strangle hydroxyl value on alcohol so rich more.Research is found, it is very excellent that richness is strangled the antioxygenic property of alcohol, but richness is strangled alcohol and is also had in actual applications some problems: 1, hydroxyl is the group relatively enlivening, and is easily activated into unstable group under other Free Radicals, causes producing certain side effect; 2, a large amount of hydroxyls in use, easily and some containing oxygen or nitrogen-containing group formation hydrogen bond, the stability of whole system is impacted; 3, to strangle alcohol performance comparatively single for richness, and range of application is limited.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of chitosan-Fu Le alcohol complex, its preparation method, moisturizing antioxidant, be intended to solve that existing richness strangles that the hydroxyl that alcohol exists is easily activated, hydroxyl and other containing oxygen or nitrogen-containing group form hydrogen bond to system stability impact, richness strangles the problem that alcohol performance is more single.
Technical scheme of the present invention is as follows:
A preparation method for chitosan-Fu Le alcohol complex, wherein, comprises step:
S1, meter in mass ratio, 80% ~ 99.5% water-soluble chitosan and 0.5% ~ 20% richness is strangled to alcohol and be dissolved in mixed solvent, and fully spinning solution is made in stirring;
S2, the spinning solution stirring is carried out to electrospinning processing;
S3, the non-woven fabrics that electrospinning processing is obtained chitosan-Fu Le alcohol complex that obtains soluble in water.
The preparation method of described chitosan-Fu Le alcohol complex, wherein, described water-soluble chitosan is using carboxyl chitosan.
The preparation method of described chitosan-Fu Le alcohol complex, wherein, described water-soluble chitosan is carboxymethyl chitosan.
The preparation method of described chitosan-Fu Le alcohol complex, wherein, in described step S2, the parameter of electrospinning processing is: voltage is 20 ~ 25KV, and receiving range is 10 ~ 15cm, and spinning solution flow velocity is 0.5 ~ 1ml/h.
The preparation method of described chitosan-Fu Le alcohol complex, wherein, in described step S1, mixing time is 5h ~ 10h.
A kind of chitosan-Fu Le alcohol complex, wherein, adopts the preparation method of arbitrary described chitosan-Fu Le alcohol complex to prepare.
A kind of moisturizing antioxidant, is characterized in that, adopting described chitosan-Fu Le alcohol complex is raw material.
Beneficial effect: the present invention carries out electrospinning processing by the mixed liquor of richness being strangled to alcohol and chitosan, from the non-woven fabrics obtaining, prepare richness and strangled alcohol-chitosan complexes, preparation method of the present invention is carried out suitable derivatization treatment by richness being strangled to alcohol, can continue richness and strangle the physiologically active of alcohol excellence, also reduce the unfavorable factor that the hydroxyl of larger amt brings, thereby expanded rich range of application and field of strangling alcohol.
Brief description of the drawings
Fig. 1 is the test pattern of the moisturizing rate of carboxymethyl chitosan.
Fig. 2 is the test pattern of the moisturizing rate of carboxymethyl chitosan-Fu Le alcohol complex.
Fig. 3 is the test pattern that does not add the blank assay of any active matter.
Fig. 4 is the test pattern that adds 50 μ L5000umol/L carboxymethyl chitosans removal free radical performances.
Fig. 5 removes free radical performance for adding 50 μ L2000umol/L carboxymethyl chitosan-Fu Le alcohol complex.
Detailed description of the invention
The invention provides a kind of chitosan-Fu Le alcohol complex, its preparation method, moisturizing antioxidant, for making object of the present invention, technical scheme and effect clearer, clear and definite, below the present invention is described in more detail.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The preparation method of chitosan-Fu Le alcohol complex provided by the invention, it comprises step:
S1, meter in mass ratio, 80% ~ 99.5% water-soluble chitosan and 0.5% ~ 20% richness is strangled to alcohol and be dissolved in mixed solvent, and fully spinning solution is made in stirring;
S2, the spinning solution stirring is carried out to electrospinning processing (electrostatic spinning processing);
S3, the non-woven fabrics that electrospinning processing is obtained chitosan-Fu Le alcohol complex that obtains soluble in water.
Water-soluble chitosan is wherein preferably using carboxyl chitosan, for example carboxymethyl chitosan, carboxymethyl chitosan has good performance of keeping humidity, and has very strong bacteriostasis, can effectively suppress the pathogenic bacterium in skin, oral cavity, tooth, so can be used as the raw material of preparation moisturizing antioxidant.
In step S1, water-soluble chitosan and richness are strangled alcohol and are dissolved in after mixed solvent, need fully stir, and the preferred mixing time of the present invention is 5h ~ 10h, fully mix with chitosan so that richness is strangled alcohol.Wherein, water-soluble chitosan with rich when strangling alcohol and mixing separately shared mass ratio be 80% ~ 99.5%, 0.5% ~ 20%.Mixed solvent wherein can be the mixed solvent of water and acetic acid, meter by volume, and the mixing ratio of water and acetic acid is 4:1.
In step S2, by the spinning solution obtaining after fully stirring, be injected into electrospinning with in syringe, then carry out electrospinning processing, the parameter of electrospinning processing is: voltage is 20 ~ 25KV, and receiving range is 10 ~ 15cm, and spinning solution flow velocity is 0.5 ~ 1ml/h.The ultimate principle of electrospinning is by by high-pressure electrostatic on spinning solution band, is with drop taylor cone summit at blood capillary under the effect of electric field of the spinning solution of point to be accelerated, and forms charged jet, is finally deposited on receptor.
Electrospinning generally realizes by electrostatic spinning apparatus, electrostatic spinning apparatus comprises the devices such as high voltage power supply, dosing pump, shower nozzle, receptor, container, ins and outs about electrostatic spinning apparatus can be with reference to content of the prior art, and the present invention no longer launches to repeat.
After electrospinning is processed, by the non-woven fabrics of collecting on the receptor brown solution that obtains soluble in water again, after removing volumetric water, can obtain chitosan-Fu Le alcohol complex, the formation principle of chitosan-Fu Le alcohol complex is: under the effect of extra electric field, chitosan and the rich hydrogen bond action of strangling between alcohol are strengthened, the hydroxyl that makes richness strangle alcohol surface is able to stabilisation, thereby the adverse effect of having avoided active hydroxyl to produce, the moisturizing antioxidant that the chitosan-Fu Le alcohol complex finally making can be used as function admirable is applied in the middle of cosmetic field.
Below by specific embodiment, the present invention is specifically described.
Embodiment mono-:
5g carboxymethyl chitosan and 50mg richness are strangled alcohol and are dissolved in (mixed solvent of 8ml water and 2ml acetic acid) in 10ml solvent, fully stir 5h, the spinning solution stirring is injected to syringe for electrospinning, regulation voltage is 20kv, receiving range is 10cm, and solution flow rate is 0.5ml/h.After switching on power, after solution to be mixed exhausts completely, the non-woven fabrics of collecting is again soluble in water, remove after volumetric water dry carboxymethyl chitosan-Fu Le alcohol complex that obtains.
Embodiment bis-:
5g carboxymethyl chitosan and 1.25g richness are strangled alcohol and are dissolved in (mixed solvent of 8ml water and 2ml acetic acid) in 10ml solvent, fully stir 10h, the spinning solution stirring is injected to syringe for electrospinning, regulation voltage is 25kv, receiving range is 15cm, and solution flow rate is 1ml/h.After switching on power, after solution to be mixed exhausts completely, the non-woven fabrics of collecting is again soluble in water, remove after aqueous solvent dry carboxymethyl chitosan-Fu Le alcohol complex that obtains.
Embodiment tri-:
The test of carboxymethyl chitosan-Fu Le alcohol complex moisture retention:
Test formula
, wherein, Si is sample moisturizing rate, %, H
n: sample is placed rear water content, H
0: sample is placed front water content.
Accurately take embodiment bis-gained 0.5g samples, after fully dry, put into the weighing botle that diameter is 3cm, adding mass fraction is the deionized water of sample size 10%, is placed in the exsiccator that dry silica gel is housed, and takes out and weigh respectively example weight in the time of placement 4,12,24,36,48,60,72,84,96h, and calculate now water content, calculate moisturizing rate according to formula, get the meansigma methods of twice experiment, and be figure.Fig. 1 is the moisturizing rate of carboxymethyl chitosan, and Fig. 2 is the moisturizing rate of carboxymethyl chitosan-Fu Le alcohol complex.From Fig. 1 and Fig. 2, can find out, the moisturizing rate of the carboxymethyl chitosan-Fu Le alcohol complex preparing does not significantly decrease with respect to carboxymethyl chitosan, so carboxymethyl chitosan-Fu Le alcohol complex also has excellent performance of keeping humidity.
Embodiment tetra-:
Carboxymethyl chitosan-Fu Le alcohol complex is removed free radical performance test
Adopt spin trapping method (ESR) to measure free radical removal effect.Concrete operations are: react the free radical producing with ferrous ion for hydrogen peroxide, utilize DMPO (5,5-dimethyl-1-pyrrolin-N-oxide) as spin trapping agent, detect the signal of the product D MPO-OH of DMPO and hydroxyl radical reaction generation.
In actual test: the concentration of green vitriol is 0.4 mmol/L, and the mass concentration of hydrogen peroxide is 5%, PBS(phosphate buffer) pH value be 7.4, C
60(OH) n-CMCS(carboxymethyl cellulose) concentration be 15 mmol/L, the concentration of DMPO is 0.4 mol/L, tests after respectively getting above five kinds of solution, 50 μ L mix homogeneously.Fig. 3 is the blank assay result that does not add any active matter, Fig. 4 is the test pattern that adds 50 μ L5000umol/L carboxymethyl chitosans removal free radical performances, Fig. 5 removes free radical performance for adding 50 μ L2000umol/L carboxymethyl chitosan-Fu Le alcohol complex (complex of embodiment mono-), wherein, abscissa represents magnetic field intensity (Gauss), and the intensity (relative intensity) of free radical is removed in vertical coordinate representative.As can be seen from the figure, the free radical removal capacity of carboxymethyl chitosan-Fu Le alcohol complex is stable, has stronger antioxidant activity.
Same method of testing, the complex in embodiment bis-, the C60-CMCS that only needs to prepare complex concentration and be 1.5mmol/l also can remove the free radical under experiment condition completely.
In sum, the present invention carries out electrospinning processing by the mixed liquor of richness being strangled to alcohol and chitosan, from the non-woven fabrics obtaining, prepare richness and strangled alcohol-chitosan complexes, preparation method of the present invention is carried out suitable derivatization treatment by richness being strangled to alcohol, can continue richness and strangle the physiologically active of alcohol excellence, also reduce the unfavorable factor that the hydroxyl of larger amt brings, thereby expanded rich range of application and field of strangling alcohol.
Should be understood that, application of the present invention is not limited to above-mentioned giving an example, and for those of ordinary skills, can be improved according to the above description or convert, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (5)
1. a preparation method for chitosan-Fu Le alcohol complex, is characterized in that, comprises step:
S1, meter in mass ratio, 80% ~ 99.5% water-soluble chitosan and 0.5% ~ 20% richness is strangled to alcohol and be dissolved in mixed solvent, and fully spinning solution is made in stirring, and mixing time is 5h ~ 10h, and described mixed solvent is the mixed solvent of water and acetic acid;
S2, the spinning solution stirring is carried out to electrospinning processing, the parameter of electrospinning processing is: voltage is 20 ~ 25KV, and receiving range is 10 ~ 15cm, and spinning solution flow velocity is 0.5 ~ 1ml/h;
S3, the non-woven fabrics that electrospinning processing is obtained chitosan-Fu Le alcohol complex that obtains soluble in water;
The formation principle of chitosan-Fu Le alcohol complex is: under the effect of extra electric field, chitosan and the rich hydrogen bond action of strangling between alcohol are strengthened, the hydroxyl that makes richness strangle alcohol surface is able to stabilisation, thereby the adverse effect of having avoided active hydroxyl to produce, the chitosan-Fu Le alcohol complex finally making is applied in the middle of cosmetic field as the moisturizing antioxidant of function admirable.
2. the preparation method of chitosan-Fu Le alcohol complex according to claim 1, is characterized in that, described water-soluble chitosan is using carboxyl chitosan.
3. the preparation method of chitosan-Fu Le alcohol complex according to claim 1, is characterized in that, described water-soluble chitosan is carboxymethyl chitosan.
4. chitosan-Fu Le alcohol complex, is characterized in that, adopts the preparation method of arbitrary described chitosan-Fu Le alcohol complex in claims 1 to 3 to prepare.
5. a moisturizing antioxidant, is characterized in that, adopting chitosan-Fu Le alcohol complex as claimed in claim 4 is raw material.
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| CN103756019B (en) * | 2013-12-19 | 2016-05-11 | 深圳市通产丽星股份有限公司 | A kind of amphipathic chitose-fullerene complex and preparation method thereof |
| CN104927069B (en) * | 2015-07-02 | 2017-07-25 | 广西南宁博恩康生物科技有限公司 | A kind of preparation method for the degradable hemostatic microsphere that can reduce pigment deposition |
| CN106757790B (en) * | 2017-01-17 | 2019-06-04 | 国家纳米科学中心 | A kind of anti-oxidant static spinning membrane and its preparation method and application |
| CN108852869B (en) * | 2018-09-04 | 2021-05-14 | 广东科玮生物技术股份有限公司 | Skin care composition for resisting blue light pollution and application thereof |
| CN110025499B (en) * | 2019-04-08 | 2021-08-17 | 大连美乐生物技术开发有限公司 | Preparation method of peony peptide-fullerene |
| CN113648463A (en) * | 2021-07-22 | 2021-11-16 | 上海市第六人民医院 | Fullerol loaded polycaprolactone nerve scaffold and preparation method thereof |
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| CN1273529C (en) * | 2002-12-20 | 2006-09-06 | 武汉大学 | Chitin mixed membrane containing Fullerene amine derivative and preparation thereof |
| CN1955213B (en) * | 2006-10-17 | 2010-09-08 | 北京服装学院 | Polymer nanofibre film mixed with fullerene and its preparation method |
| CN101239026B (en) * | 2007-12-25 | 2011-07-27 | 中国科学院上海应用物理研究所 | Application of fullerol in beauty treatment skin care products |
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Address after: No. 49, Wuhe South Road, Buji Bantian, Shenzhen, Guangdong 518112 Patentee after: Shenzhen Lihe Technology Innovation Co.,Ltd. Patentee after: PEKING University SHENZHEN GRADUATE SCHOOL Address before: No. 49, Wuhe South Road, Buji Bantian, Shenzhen, Guangdong 518112 Patentee before: SHENZHEN BEAUTY STAR Co.,Ltd. Patentee before: PEKING University SHENZHEN GRADUATE SCHOOL |
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Effective date of registration: 20210706 Address after: No. 1001, Longgang Avenue, Pingxi community, Pingdi street, Longgang District, Shenzhen, Guangdong 518000 Patentee after: Shenzhen TONGCHAN Lixing Technology Group Co.,Ltd. Patentee after: PEKING University SHENZHEN GRADUATE SCHOOL Address before: No. 49, Wuhe South Road, Buji Bantian, Shenzhen, Guangdong 518112 Patentee before: Shenzhen Lihe Technology Innovation Co.,Ltd. Patentee before: PEKING University SHENZHEN GRADUATE SCHOOL |