CN101914816B - Ferulic acid glyceryl oleate polyvinylpyrrolidone nanometer fiber membrane and preparation and application thereof - Google Patents
Ferulic acid glyceryl oleate polyvinylpyrrolidone nanometer fiber membrane and preparation and application thereof Download PDFInfo
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- CN101914816B CN101914816B CN2010102716287A CN201010271628A CN101914816B CN 101914816 B CN101914816 B CN 101914816B CN 2010102716287 A CN2010102716287 A CN 2010102716287A CN 201010271628 A CN201010271628 A CN 201010271628A CN 101914816 B CN101914816 B CN 101914816B
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- ferulic acid
- acid glyceryl
- glyceryl oleate
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- fibrous membrane
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Abstract
The invention relates to a ferulic acid glyceryl oleate polyvinylpyrrolidone nanometer fiber membrane and preparation and application thereof. The preparation comprises the following steps of: (1) adding polyvinylpyrrolidone into a solvent, adding ferulic acid glyceryl oleate with stirring, continuously stirring until solution becomes clear and performing ultrasonic degassing for 15 minutes by using an ultrasonic processor to prepare spinning solution; and (2) guiding the spinning solution into an injector, performing high-pressure electrostatic spinning under the conditions of flow rate of 0.8 to 1ml/h, distance between a receiving plate and a spinneret of 10 to 15cm, voltage of 10 to 15kV, ambient temperature of between 20 and 40 DEG C and ambient humidity of 50 to 75 percent by using a flattened needle as a capillary for injecting trickles, and performing vacuum drying for 24 hours at normal temperature to obtain the nanometer fiber membrane. The method is simple and easy to control; nano-fibers are prepared in a high-voltage electric field in one step; and the prepared fiber membrane can be used as an additive in medicine and health, food processing and daily cosmetics industries.
Description
Technical field
The invention belongs to instant nanometer tunica fibrosa field, particularly a kind of ferulic acid glyceryl oleate polyethylene is than pyrrolidone nano fibrous membrane and preparation and application.
Background technology
Forulic acid (4-hydroxyl-3-methoxy cinnamic acid; Ferulic acid; FA) be a kind of natural anti-oxidant; Extensively be present in the higher plant, its part main and polysaccharide and the crosslinked formation cell membrane of lignin, he still is one of important active ingredient of Chinese medicine asafoetide, Radix Angelicae Sinensis, Ligusticum wallichii, rattletop etc. simultaneously.Big quantity research shows that forulic acid has non-oxidizability and multiple physiologically active, thereby is widely used in fields such as medicine, food and cosmetics.But contain two keys in the forulic acid molecule, alkyl is shorter, be difficult to see through biomembrane lipid molecular layer, and the solubility in the lower aqueous solution of temperature is lower, this to a great extent limit the application of forulic acid.Through enzymatic method the forulic acid molecule has been connected with olein and can have obtained lipophilic forulic acid olein (Feruloyl-oleylglycerol; FOG), it is made up of two oleins of forulic acid and the mixing of forulic acid glyceryl monooleate.This novel structured lipid has not only overcome the short drawback of forulic acid alkyl, and because its kept forulic acid the adjusting body immunity, reduce the characteristic of multiple physiologically actives such as blood viscosity and antithrombotic and receive much concern.But the lipophilicity of this ferulic acid glyceryl oleate is very strong, in water with a lot of solvent in solubility very low, this has limited it again in a lot of Application for Field.
Polyvinylpyrrolidone (PVP) is as a kind of synthesizing water-solubility macromolecular compound; General aspects with water-soluble high-molecular compound; Colloid protective effect, film forming, caking property, hygroscopicity, solubilising or cohesion; But it is most characteristic, thereby what receive that people pay attention to is its excellent solubility property and physiological compatibility.Both water-soluble as PVP in synthetic high polymer, be dissolved in actually rare that most of organic solvent, toxicity are very low, the physiology intermiscibility is good again, particularly in medicine, food, cosmetics these and the closely-related field of health of people.His advantageous property makes it be widely used in medical and health, food processing, daily cosmetics, textile printing and dyeing, coating and fields such as pigment, polymer process.
Pass through nanometer technology; With this novel function glyceride and the strong polymer of hydrophily---polyvinylpyrrolidone combines; Can overcome the low drawback of ferulic acid glyceryl oleate solubility in the aqueous solution, the range of application of expansion ferulic acid glyceryl oleate.
Summary of the invention
Technical problem to be solved by this invention provides a kind of ferulic acid glyceryl oleate polyethylene than pyrrolidone nano fibrous membrane and preparation and application, and this method can be simple, be easy to control, and nanofiber is prepared in single step under high voltage electric field; The tunica fibrosa of preparing can be used for the additive in medical and health, food processing, the daily cosmetics industry.
A kind of ferulic acid glyceryl oleate polyethylene of the present invention is than pyrrolidone nano fibrous membrane; Comprise: a kind of ferulic acid glyceryl oleate polyethylene is than pyrrolidone nano fibrous membrane; Component comprises: 1g ferulic acid glyceryl oleate and 4~8g polyvinylpyrrolidone, diameter are 100~1250nm.
A kind of ferulic acid glyceryl oleate polyethylene of the present invention comprises than the preparation method of pyrrolidone nano fibrous membrane:
(1) 4~8g polyvinylpyrrolidone is incorporated in 40~80mL solvent, stirring condition adds the ferulic acid glyceryl oleate of 1g down, continues to be stirred to the solution becomes clarification, and ultrasonic degas was mixed with spinning solution in 15 minutes then;
(2) pouring above-mentioned spinning solution into syringe, adopt the injection needle that scabbles as the capillary that sprays thread, is 0.8~1mLh-1 at flow velocity; Receiver sheet is 10~15cm from the spinning nozzle distance; Voltage 10~15kV, environment temperature is 15~40 ℃, ambient humidity is 50~75% to carry out high-voltage electrostatic spinning; Vacuumize is 24 hours under the normal temperature, obtains nano fibrous membrane.
Polyvinylpyrrolidone in the said step (1) is K30 or K60, and ferulic acid glyceryl oleate is that two oleins of forulic acid and forulic acid glyceryl monooleate mix composition, and the two olein mol ratios of forulic acid glyceryl monooleate and forulic acid are 1: 2.
Solvent in the said step (1) is that volume ratio is 4: 1 the chloroform and the mixed solution of ethanol.
Syringe volume in the said step (2) is 5mL, and injection needle is No. 6 or No. 9.
A kind of ferulic acid glyceryl oleate polyethylene of the present invention is applied to than pyrrolidone nano fibrous membrane, as the additive of cosmetic industry, increases ferulaic acid content; Or ferulic acid glyceryl oleate polyvinylpyrrolidonenanometer nanometer fiber membrane incapsulated, be prepared into health medicine, also or through being made into paster carry out supplying human body.
Beneficial effect
(1) preparation method of the present invention is simple, and is easy to operate, is easy to control, and nanofiber is prepared in single step under high voltage electric field;
(2) the tunica fibrosa diameter of preparing is even, smooth surface, can be used for the additive in medical and health, food processing, the daily cosmetics industry.
Description of drawings
Fig. 1 is a high-voltage electrostatic spinning artwork of the present invention, and 1 is high pressure generator, and 2 is syringe pump, and 3 is flat panel collector;
Fig. 2 is the sem photograph of ferulic acid glyceryl oleate polyvinylpyrrolidonenanometer tunica fibrosa;
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.
The preparation of spinning solution:
The 1g ferulic acid glyceryl oleate is dissolved in (80: 20) in 60mL chloroform and the ethanol; Under stirring condition, add 6g polyvinylpyrrolidone K60 then; Add continued and stir 4 hours, adopted ultrasonic processor (500W) ultrasonic degas then 15 minutes until mixture change clear.
The high-pressure electrostatic spinning is equipped with instant ferulic acid glyceryl oleate nano fibrous membrane:
The solution that configures is poured in the solution storage storage (5mL syringe); No. 6 injection needles that employing is scabbled are as the capillary that sprays thread; The positive pole that connects high voltage source; Adopt aluminium foil to accept the dull and stereotyped negative pole that connects, the solution spray volume is controlled by micro-injection pump, carries out electrostatic spinning by following condition: flow velocity is 1.0mLh
-1, receiver sheet is 15cm from the spinning nozzle distance, voltage 12kV, and environment temperature is 20 ℃, ambient humidity is 65%.Fig. 1 is a high-voltage electrostatic spinning artwork of the present invention.
To spin the tunica fibrosa that comes through above-mentioned condition electricity and put into the vacuum desiccator air drying 24 hours, metal spraying is handled laggard line scanning electron microscopic observation under the vacuum then, and the result is as shown in Figure 2, and visible fibre diameter is about 1000nm.
The preparation of spinning solution:
The 1g ferulic acid glyceryl oleate is dissolved in (64: 16) in 80mL chloroform and the ethanol; Under stirring condition, add 7g polyvinylpyrrolidone K40 then; Add continued and stir 4 hours, adopted ultrasonic processor (500W) ultrasonic degas then 15 minutes until mixture change clear.
The high-pressure electrostatic spinning is equipped with instant ferulic acid glyceryl oleate nano fibrous membrane:
The solution that configures is poured in the solution storage storage (5mL syringe); No. 6 injection needles that employing is scabbled are as the capillary that sprays thread; The positive pole that connects high voltage source; Adopt aluminium foil to accept the dull and stereotyped negative pole that connects, the solution spray volume is controlled by micro-injection pump, carries out electrostatic spinning by following condition: flow velocity is 0.8mLh
-1, receiver sheet is 10cm from the spinning nozzle distance, voltage 14kV, and environment temperature is 30 ℃, ambient humidity is 55%.
To spin the tunica fibrosa that comes through above-mentioned condition electricity and put into the vacuum desiccator air drying 24 hours, metal spraying is handled laggard line scanning electron microscopic observation under the vacuum then, and fibre diameter is about 800nm.
Claims (7)
1. a ferulic acid glyceryl oleate polyethylene is than pyrrolidone nano fibrous membrane, and component comprises: 1g ferulic acid glyceryl oleate and 4~8g polyvinylpyrrolidone, diameter are 100~1250nm;
The preparation method of this nano fibrous membrane comprises:
(1) 4~8g polyvinylpyrrolidone is incorporated in 40~80mL solvent, stirring condition adds the ferulic acid glyceryl oleate of 1g down, continues to be stirred to the solution becomes clarification, and ultrasonic degas was mixed with spinning solution in 15 minutes then;
(2) pouring above-mentioned spinning solution into syringe, adopt the injection needle that scabbles as the capillary that sprays thread, is 0.8~1mLh at flow velocity
-1, receiver sheet is 10~15cm from spinning nozzle distance, voltage 10~15kV, and environment temperature is 15~40 ℃, and ambient humidity is 50~75% to carry out high-voltage electrostatic spinning, and vacuumize is 24 hours under the normal temperature, obtains nano fibrous membrane.
2. a kind of ferulic acid glyceryl oleate polyethylene according to claim 1 is than pyrrolidone nano fibrous membrane; It is characterized in that: the ferulic acid glyceryl oleate in said preparation method's the step (1) is two oleins of forulic acid and forulic acid glyceryl monooleate mixture, and the two olein mol ratios of forulic acid glyceryl monooleate and forulic acid are 1: 2.
3. a kind of ferulic acid glyceryl oleate polyethylene according to claim 1 is characterized in that than pyrrolidone nano fibrous membrane: the solvent in said preparation method's the step (1) is that volume ratio is 4: 1 the chloroform and the mixed solution of ethanol.
4. a kind of ferulic acid glyceryl oleate polyethylene according to claim 1 is characterized in that than pyrrolidone nano fibrous membrane: the syringe volume in said preparation method's the step (2) is 5mL, and injection needle is No. 6 or No. 9.
5. a kind of ferulic acid glyceryl oleate polyethylene as claimed in claim 1 is than the application of pyrrolidone nano fibrous membrane; It is characterized in that: with the ferulic acid glyceryl oleate polyethylene than the additive of pyrrolidone nano fibrous membrane, to increase content of ferulic acid as cosmetic industry.
6. a kind of ferulic acid glyceryl oleate polyethylene as claimed in claim 1 is characterized in that: ferulic acid glyceryl oleate polyvinylpyrrolidonenanometer nanometer fiber membrane is incapsulated, be prepared into health medicine than the application of pyrrolidone nano fibrous membrane.
7. a kind of ferulic acid glyceryl oleate polyethylene as claimed in claim 1 is characterized in that than the application of pyrrolidone nano fibrous membrane: ferulic acid glyceryl oleate polyvinylpyrrolidonenanometer nanometer fiber membrane is made into paster carries out supplying human body.
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CN102864503B (en) * | 2012-10-10 | 2014-10-15 | 青岛大学 | Electrostatic spinning device for scale production of micro-nano-fiber |
CN103445973A (en) * | 2013-09-09 | 2013-12-18 | 中山大学 | Nano fiber whitening and freckle-removing mask paste |
CN104862817A (en) * | 2015-06-02 | 2015-08-26 | 天津工业大学 | Preparation method of health-care fiber containing nanometer selenium |
CN106149195B (en) * | 2016-08-18 | 2018-05-15 | 华南理工大学 | Nano fibrous membrane that is a kind of while embedding fish oil and forulic acid and preparation and application |
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JP2007314914A (en) * | 2006-05-26 | 2007-12-06 | Suzuki Kutsushita:Kk | Chemical fiber containing rice bran oil and textile product using the same |
CN101328646A (en) * | 2008-06-20 | 2008-12-24 | 东华大学 | Preparation of ultravioresistant nonwoven |
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JP2007314914A (en) * | 2006-05-26 | 2007-12-06 | Suzuki Kutsushita:Kk | Chemical fiber containing rice bran oil and textile product using the same |
CN101328646A (en) * | 2008-06-20 | 2008-12-24 | 东华大学 | Preparation of ultravioresistant nonwoven |
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