CN102560887A - Silk fibroin nano-fiber film loaded with vitamins A and E and preparation method thereof - Google Patents
Silk fibroin nano-fiber film loaded with vitamins A and E and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a silk fibroin nano-fiber film loaded with vitamins A and E and a preparation method thereof. The nano-fiber film comprises silk fibroin nano-fiber, as well as the fat-soluble vitamin A and the water-soluble vitamin E, which are loaded in the silk fibroin nano-fiber. The preparation method comprises the following steps of: (1) heating the vitamins A and E till melting, uniformly stirring, then adding deionized water at the temperature of 80-100 DEG C, and stirring for 10-20min till transparent liquid, namely an emulsion of the vitamins A and E, is formed; (2) adding silk fibroin and the deionized water into the emulsion of the vitamins A and E till the final concentration, and stirring till the complete solution of the silk fibroin so as to get a mixed solution of the three; and (3) transferring the solution into a syringe for performing electrostatic spinning to get the silk fibroin nano-fiber film. The silk fibroin nano-fiber film disclosed by the invention has the advantages of no pollution, low cost and simple operation, and the nano-fiber disclosed by the invention can be applied to artificial skin, medical dressings, hemostatic materials, skin care products and other various biomedical fields.
Description
Technical field
The invention belongs to silk fibroin nano-fiber film and preparation field thereof, silk fibroin nano-fiber film of particularly a kind of load vitamin A and E and preparation method thereof.
Background technology
Nanofiber has broad application prospects at biomedical sector owing to have that yardstick is little, specific area is big and characteristics such as physical property excellence.Nano fibrous membrane has little aperture and high specific area can promote hemostasis reaction and without styptic.The nano fibrous membrane loose structure helps the breathing of cell and does not cause that wound is dry, and little aperture effectively stops the bacterium intrusion simultaneously, has the high ventilation oxygen permeability again.Change dressings brings the probability that disturbs nerve fiber regeneration.Electrostatic spinning nano fiber can be given the better self-regeneration of Skin Cell path, and from the viewpoint of organizational project, bionical nanofibrous structures has good cell conductibility and the compatibility of improving blood, and wound is healed and skin regeneration more easily.Nanofiber still is the ideal material of encapsulated drug, and it not only can be encapsulated into solid drugs in the fiber with particle form, can also liquid medicine be encapsulated with double-deck fiber or chain pearl fibers form, thereby effectively realize controlled delivery of pharmaceutical agents is discharged.Because fibroin albumen is the profuse native protein of a kind of nature, have excellent performance such as excellent biological compatibility, biodegradability, high ventilation, poisture-penetrability, non-immunogenicity, be widely used in biomedicine field in recent years.
Multivitamin comes to light and skin health has substantial connection, in patent CN 101736430 A, has just announced that a kind of load has the preparation method of ascorbic silk fibroin nano-fiber, and its fiber has skin-care effect.Vitamin A is a kind of liposoluble substance, can make the epithelium organ keep eubolism.The ultraviolet ray of the sun can cause the vitamin(e) A deficiency in the human body skin; And possibly cause the early ageing and the cutaneum carcinoma of skin, if can reduce the destruction of ultraviolet ray to skin greatly with vitamin A preliminary treatment skin, so vitamin A has the effect of minimizing by light aging; Vitamin A also can be treated acute promyelocytic leukemia; Acne and other skin skin disorders, and the skin aging that can slow down are removed wrinkle.The stability problem of vitamin A is not solved at present at home yet.Many producers contain in the aqueous solution preparation process of vitamin A in making, taked such as regulator solution pH value, add complexing agent and remove measure such as filling CO 2 in metal ion, the finished product, stabilizing vitamin A.Vitamin E is called anti-infertility vitamin or tocopherol again, is a kind of transparent faint yellow thickness grease, and is water insoluble, is dissolved in organic solvent, and soda acid hydrogenation process and high temperature all can not destroy vitamin E.But it is the meeting eremacausis in air, and ultraviolet irradiation can make its decomposition.It can be protected other to be prone to oxidized material and it is not destroyed, so it is extremely effective oxidant, can prevent heavy metal, produces the hepatotoxin of free radical and can cause the various medicines infringements that oxidant is caused injury.Polyethylene glycol VE-succinate (D-α-tocopherol polyethylene glycol succinate; TPGS; Vitamin E TPGS; Tocophersolan) be the soluble derivative of vitamin E, form loaded " American Pharmacopeia " by the carboxyl and polyethylene glycol (PEG) esterification of VE-succinate (VES).TPGS is produced and listing by U.S. Eastman company the earliest; Be widely used in the preparation research abroad at present; Carrier as solubilizer, sorbefacient, emulsifying agent, plasticizer and slightly water-soluble and fat-soluble medicine transmission system; Like the carrier of administration in the carrier of solid dispersions, dosing eyes, the nasal cavity etc., existing at present TPG (mass fraction is 20% the aqueous solution) launch of the U.S. is (like Mazuri
TM), as the nutritious supplementary pharmaceutical of vitamin E, amount to into vitamin E and tire and be about 77.4IUg
-1TPGS is highly stable, and room temperature is placed not hydrolysis, and almost tasteless, can be used as people's vitamin E replenishers, and particularly those are absorbed with the people of obstacle to liposoluble vitamin E.In US 523469;, compare with taking liposoluble vitamin E as animal subject with elephant and African elephant, oral mass fraction is behind 20% the TPGS solution; Vitamin E concentration increases soon in the body, just can reach higher blood concentration than the watermiscible vitamin E of low dosage.
Summary of the invention
Technical problem to be solved by this invention provides silk fibroin nano-fiber film of a kind of load vitamin A and E and preparation method thereof; A plurality of biomedicine fields such as this silk fibroin nano-fiber film using artificial skin, medical dressing, hemostatic material, skin-protection product; In whole process of preparation of the present invention, do not relate to any to environment and the disagreeableness material of human health, pollution-free; Cost is low, and is simple to operate.
The silk fibroin nano-fiber film of a kind of load vitamin A of the present invention and E; Said nano fibrous membrane comprises silk fibroin nano-fiber and is carried on fat-soluble A and the watermiscible vitamin E in the silk fibroin nano-fiber that the diameter of nano fibrous membrane is 10-800nm.
Said watermiscible vitamin E is a vitamin E polyethylene glycol succinic acid ester.
Said fat-soluble A is Retinol Palmitate or vitamin(e) A acetate.
The diameter of said nano fibrous membrane is 300-600nm.
The preparation method of the silk fibroin nano-fiber film of a kind of load vitamin A of the present invention and E comprises:
(1) fat-soluble A and watermiscible vitamin E are heated to thawing, stir,, stir 10-20min to transparency liquid, i.e. vitamin A and E emulsion subsequently in the deionized water of 80～100 ℃ of addings with respect to vitamin E quality 4-9 times;
(2) in said vitamin A and E emulsion, add fibroin albumen and deionized water to final concentration, be stirred to fibroin albumen and dissolve fully, get fibroin albumen-vitamin A-vitamin E solution; Wherein, the final concentration of vitamin E is 0.1-2wt%, and the final concentration of fibroin albumen is 20-35wt%, and the final concentration of vitamin A is 0.1-8wt%;
(3) with carrying out electrostatic spinning in above-mentioned fibroin albumen-vitamin A-vitamin E solution immigration syringe, promptly get the silk fibroin nano-fiber film.
The preparation method of the fibroin albumen in the said step (2) is: will go the pupa silk cocoon at 100 ℃ 0.5wt%Na
2CO
3Boil 2-5 time in the aqueous solution, each 30min comes unstuck, and obtains fibroin, and the use mol ratio is 1: 2: 8 CaCl
2, C
2H
5OH and H
2O or with the 0.8g/ml LiBr aqueous solution 40-60 ℃ the dissolving 1-2h, with distill water dialysis 3-5 days, freeze drying promptly got.
The final concentration of the vitamin E in the said step (2) is 0.5-2wt%.
The final concentration of the fibroin albumen in the said step (2) is 25-30wt%.
The final concentration of the vitamin A in the said step (2) is 0.5-8wt%.
The process conditions of the electrostatic spinning in the said step (3) are: electrostatic pressure is the 16-20 kilovolt, and accepting distance is 80-220mm, spinning speed be the 0.1-1.0 milliliter/hour.
The present invention uses TPGS as emulsifying agent, the vitamin A load is gone in the nanofiber, thereby the protection vitamin A improves the utilization rate of medicine, reduces dosage, reduces and prevents the injury of medicine to other positions of health, reduces the burden of metabolic system simultaneously.
Beneficial effect
The present invention can make vitamin A, vitamin E and fibroin albumen be dissolved in the water simultaneously; In whole process of preparation of the present invention, do not relate to any to environment and the disagreeableness material of human health, pollution-free; Cost is low; Simple to operate, and combine to utilize the good characteristics of nanofiber, vitamin A and E and fibroin albumen, but load of the present invention has a plurality of biomedicine fields such as the nanofiber using artificial skin, medical dressing, hemostatic material, skin-protection product of Solvisyn-A and E.
Description of drawings
Fig. 1 is the sem photograph of embodiment 1 prepared micro/nano fibrous membrane material;
Fig. 2 is the sem photograph of embodiment 2 prepared micro/nano fibrous membrane materials;
Fig. 3 is the sem photograph of embodiment 3 prepared micro/nano fibrous membrane materials;
Fig. 4 is the fiber diameter distribution profile of the micro/nano fibrous membrane material of embodiment 1 gained;
Fig. 5 spins vitamin A-vitamin E silk fibroin nano-fiber support proliferative activity relatively for fibroblast in emulsion;
Fig. 6 spins vitamin A-vitamin E nano fibrous framework cell antioxygenic property relatively for emulsion.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
(1) will go the pupa silk cocoon at 100 ℃ 0.5wt%Na
2CO
3Boil in the aqueous solution 2 times, each 30min comes unstuck, and will come unstuck obtains fibroin, and the use mol ratio is 1: 2: 8 CaCl
2, C
2H
5OH and H
2O is at 60 ℃ of dissolving 1.5h, the cellular solid filament fibroin that freeze drying obtains loosening.
(2) accurately take by weighing 0.16 gram TPGS and 0.02 gram Retinol Palmitate, be heated to thawing, magnetic agitation is even; Heat 90 ℃ the deionized water of 1.44ml subsequently, fully stir 15min, remove thermal source; Be stirred to and be transparent, little yellow liquid, in vitamin A-vitamin E emulsion, add 1.0g fibroin albumen and deionized water, final mass is 4.0g; The sealing continued is stirred to fibroin albumen and dissolves fully, leaves standstill subsequently after several minutes spinning solution is transferred in the syringe, and voltage is 20kV; The syringe pump fltting speed is 0.3ml/h, adopts aluminium foil to receive, and receiving range is 18cm;, the silk fibroin nano-fiber film of load vitamin A and E, average diameter is 465 ± 161nm.
Embodiment 2
(1) will go the pupa silk cocoon at 100 ℃ 0.5wt%Na
2CO
3Boil in the aqueous solution 4 times, each 30min comes unstuck, and will come unstuck obtains fibroin, and the 0.8g/ml LiBr aqueous solution is at 45 ℃ of dissolving 2h, the cellular solid filament fibroin that freeze drying obtains loosening.
(2) accurately take by weighing 0.32 gram TPGS and 0.08 gram Retinol Palmitate, be heated to thawing, magnetic agitation is even; Heat 90 ℃ the deionized water of 1.2ml subsequently, fully stir 15min, remove thermal source; Be stirred to and be transparent, little yellow liquid, in vitamin A-vitamin E emulsion, add 1.0g fibroin albumen and deionized water, final mass is 4.0g; The sealing continued is stirred to fibroin albumen and dissolves fully, leaves standstill subsequently after several minutes spinning solution is transferred in the syringe, and voltage is 18kV; The syringe pump fltting speed is 04ml/h, adopts aluminium foil to receive, and receiving range is 18cm;, the silk fibroin nano-fiber film of load vitamin A and E, average diameter is 405 ± 110nm.
(1) will go the pupa silk cocoon at 100 ℃ 0.5wt%Na
2CO
3Boil in the aqueous solution 5 times, each 30min comes unstuck, and will come unstuck obtains fibroin, and the 0.8g/ml LiBr aqueous solution is at 45 ℃ of dissolving 2h, the cellular solid filament fibroin that freeze drying obtains loosening.
(2) accurately take by weighing 0.016 gram TPGS and 0.04 gram Retinol Palmitate, be heated to thawing, magnetic agitation is even, heats 85 ℃ the deionized water of 1.2ml subsequently; Fully stirring 15min removes thermal source, is stirred to be transparent, little yellow liquid; In vitamin A-vitamin E emulsion, add 1.5g fibroin albumen and deionized water, final mass is 4.0g, and the sealing continued is stirred to fibroin albumen and dissolves fully; Leave standstill subsequently after several minutes spinning solution is transferred in the syringe, voltage is 18kV, and the syringe pump fltting speed is 0.4ml/h; The employing aluminium foil receives, and receiving range is 18cm, gets the silk fibroin nano-fiber film of load vitamin A and E.
Embodiment 4
(1) will go the pupa silk cocoon at 100 ℃ 0.5wt%Na
2CO
3Boil in the aqueous solution 5 times, each 30min comes unstuck, and will come unstuck obtains fibroin, and the 0.8g/ml LiBr aqueous solution is at 40 ℃ of dissolving 1h, the cellular solid filament fibroin that freeze drying obtains loosening.
(2) accurately take by weighing 0.32 gram TPGS and 0.08 gram Retinol Palmitate, be heated to thawing, magnetic agitation is even, heats 90 ℃ the deionized water of 1.2ml subsequently; Fully stirring 15min removes thermal source, is stirred to be transparent, little yellow liquid; In vitamin A-vitamin E emulsion, add 0.8g fibroin albumen and deionized water, final mass is 4.0g, and the sealing continued is stirred to fibroin albumen and dissolves fully; Leave standstill subsequently after several minutes spinning solution is transferred in the syringe, voltage is 20kV, and the syringe pump fltting speed is 1ml/h; The employing aluminium foil receives, and receiving range is 22cm, gets the silk fibroin nano-fiber film of load vitamin A and E.
(1) will go the pupa silk cocoon at 100 ℃ 0.5wt%Na
2CO
3Boil in the aqueous solution 5 times, each 30min comes unstuck, and will come unstuck obtains fibroin, and the 0.8g/ml LiBr aqueous solution is at 45 ℃ of dissolving 2h, the cellular solid filament fibroin that freeze drying obtains loosening.
(2) accurately take by weighing 0.32 gram TPGS and 0.02 gram Retinol Palmitate, be heated to thawing, magnetic agitation is even, heats 90 ℃ the deionized water of 1.38ml subsequently; Fully stirring 15min removes thermal source, is stirred to be transparent, little yellow liquid; In vitamin A-vitamin E emulsion, add 0.8g fibroin albumen and deionized water, final mass is 4.0g, and the sealing continued is stirred to fibroin albumen and dissolves fully; Leave standstill subsequently after several minutes spinning solution is transferred in the syringe, voltage is 16kV, and the syringe pump fltting speed is 1ml/h; The employing aluminium foil receives, and receiving range is 0.8cm, gets the silk fibroin nano-fiber film of load vitamin A and E.
Effect embodiment 1
Biocompatibility detects
(1) material preparation and processing
Like previous embodiment 1; 2 method obtain solutions also adopt other spinning parameters in embodiment 1,2 method, and adopting diameter is the circular lid slide reception electrostatic spinning nano fiber of 14mm; Be positioned in the vacuum drying chamber tunica fibrosa dry; Place 75% (v/v) alcohol vapour 24h, carry out the post processing and the sterilization of material, be used for cellular incubation.
Wherein: service property (quality) concentration is 25% pure silk fibroin spinning solution; Voltage is 20kV, and the syringe pump fltting speed is 0.3ml/h, and adopting diameter is the circular lid slide reception electrostatic spinning nano fiber of 14mm; Receiving range is 18cm, as a comparison the nanofiber group among the embodiment 1.Adopt the circular lid slide of 14mm, as a comparison the slide group among the embodiment 2.
Control group places 75% (v/v) alcohol vapour 24h equally, carries out the post processing and the sterilization of material, is used for cellular incubation.
(2) MTT experiment
With 10
4The fibroblast suspension inoculation of individual/mL is the embodiment 1,2,3 and comparative example 1,2 through sterilizing in 24 well culture plates, every hole inoculating cell suspension 200 μ L, every group 3 hole.After cultivating 1d, 3d, 5d and 7d respectively; Every group 3 hole changed and added nutrient solution 360 μ L and MTT solution (5mg/mL) the 40 μ L that do not contain serum, and incubator is cultivated 3～4h, inhales and removes nutrient solution in the hole; Every hole adds 400 μ L dimethyl sulfoxide (DMSO)s, and vibration 30min makes the crystal dissolving.Every hole is got dmso solution liquid 100 μ L and is added in the 96 hole ELISA Plates, on ELIASA, surveys the OD value with the 492nm wavelength period then.Establish 3 multiple holes for every group, and repeated experiments 3 times.The result is shown in accompanying drawing 5:
The MTT effect:
Accompanying drawing 5 is for being depicted as the propagation situation that fibroblast was cultivated 1,3,5,7 day on the nano fiber scaffold under different vitamin As and the vitamin E concentration.Compare (comparative example 2) with slide, cell all has better propagation on the electrostatic spinning nano fiber support.It should be noted that embodiment 1 nano fiber scaffold because its fibre structure is more mellow and full evenly, the propagation that more is of value to cell adheres to.And embodiment 2 nanofibers are more owing to beading quantity, and fibre structure is irregular, and the activity of its cell proliferation is lower than two groups of nano fiber scaffolds (embodiment 1 and comparative example 1) in addition.Hence one can see that, and the concentration proportioning of vitamin A and vitamin E is non-obvious, and the delicate variation of component also can cause the difference of biocompatibility effect.Cultivate after 7 days; Cell has in load that (embodiment 1 on the plain nano fiber scaffold of vitamin and pure silk; 2 and comparative example 1) propagation obviously faster than the slide group, have significant difference (P＜0.05), and also have significant difference (P＜0.05) between each nanofiber group.Hence one can see that, and emulsion is spun vitamin fibroin albumen composite nano fiber and had good biocompatibility, and the nanofiber group among the embodiment 1, and biocompatibility is superior to embodiment 2.
Effect embodiment 2
Antioxygenic property:
Cell reaches 90% (the growth area covers about 90%) by being cultured to degrees of fusion on the laboratory routine operation inoculation material, adds the oxidant t-BHP (50,100,200 of variable concentrations; 400 μ M), co-incubation 24 hours uses the PBS buffer solution to wash subsequently 3 times; Every hole adds the DMEM culture medium 360 μ L of preheating, and the MTT 40 μ L that add preheating then continue to cultivate the sucking-off culture medium 4 hours; Every hole adds DMSO 400 μ L, in 37 ℃ of shaking tables, dissolves 20min, forms purple solution; Add in 96 well culture plates with the liquid-transfering gun draw solution then, every hole 100 μ L measure light absorption value.
Anti-oxidant result:
T-BHP can induce fibroblastic cellular damage and apoptosis, the model of oxidative of doing commonly used, and whether the silk fibroin nano-fiber support that present embodiment is investigated load vitamin helps Skin Cell to resist the oxidative damage that t-BHP causes.
Be cultured to degrees of fusion after cell is inoculated by the method in the aforementioned MTT experiment and reach 90% (degree that is paved with of cell), add the oxidant t-BHP (50,100,200 of variable concentrations; 400 μ M), co-incubation 24 hours uses the PBS buffer solution to wash subsequently 3 times; Every hole adds the DMEM culture medium 360 μ L of preheating, and the MTT 40 μ L that add preheating then continue to cultivate the sucking-off culture medium 4 hours; Every hole adds DMSO 400 μ L, in 37 ℃ of shaking tables, dissolves 20min, forms purple solution; Add in 96 well culture plates with the liquid-transfering gun draw solution then, every hole 100 μ L measure light absorption value.The result is shown in accompanying drawing 6:
As shown in Figure 6, the SF vigor on the slide control group (comparative example 2) is along with the increase of t-BHP concentration presents remarkable decline trend.The t-BHP of low concentration (50-100 μ M) spins the not infringement of cell on vitamin A-vitamin E silk fibroin nano-fiber support to embodiment 1 prepared emulsion; Increased its activity (comparing) on the contrary slightly with the pure culture base group of not adding t-BHP; When t-BHP concentration increases to 200 μ M when above, cell activity still remains on about 85% and (compares with the pure culture base group of not adding t-BHP).And the plain nanofiber group of pure silk (comparative example 1) is relatively poor to the tolerance of high concentration (400 μ M) t-BHP, and cytoactive is merely about 70%, shows that its antioxidant effect spins vitamin (A-E) nanofiber group not as good as emulsion.The antioxidation of vitamin E is known dawn already, and vitamin A can react with the phenol oxygen radical, thereby plays oxidation resistant effect effectively.Above-mentioned vitamin A-vitamin E the silk fibroin nano-fiber that shows helps SF to anti-oxidative damage.
Claims (10)
1. the silk fibroin nano-fiber film of load vitamin A and E; It is characterized in that: said nano fibrous membrane comprises silk fibroin nano-fiber and is carried on fat-soluble A and the watermiscible vitamin E in the silk fibroin nano-fiber that the diameter of nano fibrous membrane is 10-800nm.
2. the silk fibroin nano-fiber film of a kind of load vitamin A according to claim 1 and E is characterized in that: said watermiscible vitamin E is a vitamin E polyethylene glycol succinic acid ester.
3. the silk fibroin nano-fiber film of a kind of load vitamin A according to claim 1 and E is characterized in that: said fat-soluble A is Retinol Palmitate or vitamin(e) A acetate.
4. the silk fibroin nano-fiber film of a kind of load vitamin A according to claim 1 and E is characterized in that: the diameter of said nano fibrous membrane is 300-600nm.
5. the preparation method of the silk fibroin nano-fiber film of load vitamin A and E comprises:
(1) fat-soluble A and watermiscible vitamin E are heated to thawing, stir,, stir 10-20min to transparency liquid, i.e. vitamin A and E emulsion subsequently in the deionized water of 80～100 ℃ of addings with respect to vitamin E quality 4-9 times;
(2) in said vitamin A and E emulsion, add fibroin albumen and deionized water to final concentration, be stirred to fibroin albumen and dissolve fully, get fibroin albumen-vitamin A-vitamin E solution; Wherein, the final concentration of vitamin E is 0.1-2wt%, and the final concentration of fibroin albumen is 20-35wt%, and the final concentration of vitamin A is 0.1-8wt%;
(3) with carrying out electrostatic spinning in above-mentioned fibroin albumen-vitamin A-vitamin E solution immigration syringe, promptly get the silk fibroin nano-fiber film.
6. the preparation method of the silk fibroin nano-fiber film of a kind of load vitamin A according to claim 5 and E is characterized in that: the preparation method of the fibroin albumen in the said step (2) is: will go the pupa silk cocoon at 100 ℃ 0.5wt%Na
2CO
3Boil 2-5 time in the aqueous solution, each 30min comes unstuck, and obtains fibroin, and the use mol ratio is 1: 2: 8 CaCl
2, C
2H
5OH and H
2O or with the 0.8g/ml LiBr aqueous solution 40-60 ℃ the dissolving 1-2h, with distill water dialysis 3-5 days, freeze drying promptly got.
7. the preparation method of the silk fibroin nano-fiber film of a kind of load vitamin A according to claim 5 and E is characterized in that: the final concentration of the vitamin E in the said step (2) is 0.5-2wt%.
8. the preparation method of the silk fibroin nano-fiber film of a kind of load vitamin A according to claim 5 and E is characterized in that: the final concentration of the fibroin albumen in the said step (2) is 25-30wt%.
9. the preparation method of the silk fibroin nano-fiber film of a kind of load vitamin A according to claim 5 and E is characterized in that: the final concentration of the vitamin A in the said step (2) is 0.5-8wt%.
10. the preparation method of the silk fibroin nano-fiber film of a kind of load vitamin A according to claim 5 and E; It is characterized in that: the process conditions of the electrostatic spinning in the said step (3) are: electrostatic pressure is the 16-20 kilovolt; Accepting distance is 80-220mm, spinning speed be the 0.1-1.0 milliliter/hour.
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