CN117188038A - Alcohol soluble protein nanofiber membrane and preparation method thereof - Google Patents
Alcohol soluble protein nanofiber membrane and preparation method thereof Download PDFInfo
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- CN117188038A CN117188038A CN202311151983.4A CN202311151983A CN117188038A CN 117188038 A CN117188038 A CN 117188038A CN 202311151983 A CN202311151983 A CN 202311151983A CN 117188038 A CN117188038 A CN 117188038A
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- highland barley
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- zein
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- 239000012528 membrane Substances 0.000 title claims abstract description 27
- 239000002121 nanofiber Substances 0.000 title claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 17
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 235000007340 Hordeum vulgare Nutrition 0.000 claims abstract description 21
- 229920002494 Zein Polymers 0.000 claims abstract description 14
- 239000005019 zein Substances 0.000 claims abstract description 14
- 229940093612 zein Drugs 0.000 claims abstract description 14
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 6
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 6
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- 241000209219 Hordeum Species 0.000 claims description 20
- 108060006613 prolamin Proteins 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 235000013339 cereals Nutrition 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000000861 blow drying Methods 0.000 claims 1
- 238000005485 electric heating Methods 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002657 fibrous material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 240000005979 Hordeum vulgare Species 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 6
- 238000001523 electrospinning Methods 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 description 2
- 239000005770 Eugenol Substances 0.000 description 2
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 229960002217 eugenol Drugs 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 239000001963 growth medium Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 1
- 239000001116 FEMA 4028 Substances 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 1
- 235000011175 beta-cyclodextrine Nutrition 0.000 description 1
- 229960004853 betadex Drugs 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000010794 food waste Substances 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The invention belongs to the field of fiber material synthesis, and particularly relates to an alcohol soluble protein nanofiber membrane and a preparation method thereof. According to the invention, after zein and highland barley zein are compounded according to a certain proportion, cyclodextrin is added into the zein, and the mechanical strength, the slow release performance and the barrier performance of the nanofiber membrane formed after electrostatic spinning can be greatly improved.
Description
Technical Field
The invention belongs to the field of fiber material synthesis, and particularly relates to an alcohol soluble protein nanofiber membrane and a preparation method thereof.
Background
Packaging plays a key role in protecting food, prolonging the shelf life of food and reducing food waste. Synthetic plastics are widely used for food packaging due to their high mechanical strength, high barrier properties, low cost, etc., but their toxicity, nondegradabilities, raw (petroleum) costs, etc. have limited their application in the field of food packaging. The edible film is used as a green packaging material, has wide raw material sources, has the advantages of incomparable safety and zero waste of other materials, and has good development prospect.
The current preparation of novel degradable films consists of proteins, lipids, polysaccharides or their complexes, the inherent properties of proteins make them an excellent choice for the production of edible films. The nanofiber membrane has extremely high specific surface area, barrier property and high slow release performance of antibacterial substances, however, the edible fiber membrane formed by using macromolecules such as protein, polysaccharide and the like has the biggest defects of low mechanical strength and poor water resistance, and greatly limits the application of the nanofiber membrane.
The prolamine is a degradable water-insoluble protein, can form an ideal nanofiber membrane, and is used as a main raw material to prepare the nanofiber material by compounding at home and abroad. However, the nanofiber membrane has the main characteristics of high brittleness, low mechanical strength, water resistance and slow release performance, and is difficult to meet the requirements.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of highland barley prolamin, which comprises the steps of drying highland barley distillers' grains in an electric drying box, crushing and sieving a dried sample; adding the sample powder into ethanol water solution, stirring with a magnetic stirrer, and heating in water bath for 120 min; and centrifuging the solution, adding water into the supernatant, precipitating, centrifuging, collecting the precipitate, and freeze-drying to obtain the target product.
Further, the screen is a 40 mesh screen.
Further, the aqueous ethanol solution is a 75% aqueous ethanol solution.
Further, the water bath heating temperature is 30-50 ℃.
Further, the centrifugation step is specifically centrifugation at 5000g for 15min.
The invention also provides highland barley alcohol soluble protein which is prepared by the preparation method.
The invention also provides an alcohol soluble protein nanofiber membrane which comprises the following components in parts by mass: 15-20% of zein, 5-10% of highland barley zein, 2-3% of glycerol, 3-7% of cyclodextrin and the balance of acetic acid.
Further, the highland barley prolamin is the highland barley prolamin.
The invention also provides a preparation method of the prolamine nanofiber membrane, which comprises the steps of uniformly mixing the components according to the proportion, wherein the total protein content is 25%, and preparing the electrospun membrane on an electrospinning machine.
Further, the voltage of the electrostatic spinning machine is 17kV, and the distance from the needle point to the collector electrode is kept at 13cm.
The invention has the following beneficial effects:
according to the invention, after zein and highland barley prolamine are compounded, the stretching rate, the mechanical strength, the slow release performance and the barrier performance are obviously improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 example 1 fibrous membrane;
FIG. 2 example 2 fibrous membrane;
FIG. 3 comparative example 1 fibrous membrane;
FIG. 4 comparative example 2 fibrous membrane;
fig. 5 comparative example 3 fibrous membrane.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, with reference to the examples using conventional methods, unless otherwise indicated, and with reference to reagents, either conventional commercial reagents or reagents configured using conventional methods. The detailed description is not to be taken as limiting, but is to be understood as a more detailed description of certain aspects, features, and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Preparation of highland barley alcohol soluble protein: the highland barley distillers' grains are dried in an electric drying box (DHG-9070B, jinan, china) at 70 ℃ until the weight is fixed. The dried sample was crushed and passed through a 40 mesh screen. 100 g of the powder was added to 1000ml of 75% aqueous ethanol and stirred with a magnetic stirrer for 5 minutes [29,30]. The samples were then heated in a 40℃water bath (HH-S6, jinan, china) for 120 minutes. The solution was centrifuged at 5000g for 15min, the supernatant was poured into a 20L stainless steel pan, and 8L of water was added to precipitate highland barley prolamin. The mixture was centrifuged at 5000g for 15min, and the precipitate was collected and lyophilized to a fixed weight.
Zein is purchased from sigma company; beta-cyclodextrin was purchased from a company of ala Ding Shiji.
Example 1: zein and highland barley prolamin are mixed according to the mass ratio of 6:4 to acetic acid containing 2.5% glycerol and 5% cyclodextrin, wherein the total protein concentration is 25%. The nanofibers were prepared on an electrospinning machine (HZ-11) with a voltage of 17kV and a tip-to-collector distance of 13cm under magnetic stirring (500 rpm) at room temperature for 30min, and the electrospun film was peeled off for use.
Example 2: zein and highland barley prolamin are mixed according to the mass ratio of 8:2 to acetic acid containing 2.5% glycerol and 8% cyclodextrin, wherein the total protein concentration is 25%. The nanofibers were prepared on an electrospinning machine (HZ-11) with a voltage of 17kV and a tip-to-collector distance of 13cm under magnetic stirring (500 rpm) at room temperature for 30min, and the electrospun film was peeled off for use.
Comparative example 1: zein and highland barley prolamin are mixed according to the mass ratio of 6:4 was added to acetic acid containing 2.5% glycerol to give a total protein concentration of 25%. The nanofibers were prepared on an electrospinning machine (HZ-11) with a voltage of 17kV and a tip-to-collector distance of 13cm under magnetic stirring (500 rpm) at room temperature for 30min, and the electrospun film was peeled off for use.
Comparative example 2: zein was added to acetic acid containing 2.5% glycerol at a total protein concentration of 25%. The nanofibers were prepared on an electrospinning machine (HZ-11) with a voltage of 17kV and a tip-to-collector distance of 13cm under magnetic stirring (500 rpm) at room temperature for 30min, and the electrospun film was peeled off for use.
Comparative example 3: zein and highland barley prolamin are mixed according to the mass ratio of 6:4 was added to acetic acid containing 2.5% glycerol, wherein the total protein concentration was 25%. The nanofibers were prepared on an electrospinning machine (HZ-11) with a voltage of 17kV and a tip-to-collector distance of 13cm under magnetic stirring (500 rpm) at room temperature for 30min, and the electrospun film was peeled off for use.
Test example:
mechanical property test: the fiber film was cut into a 5mm by 30mm bar, and a tensile test was performed using a yarn fiber extensometer, with a holding length of 10mm and a tensile speed of 10mm/min.
Morphology testing: observations were made using a scanning electron microscope model hitachit SU1510, manufactured by japanese Hitachi.
Wettability test: the static contact angle of the fibrous film was measured using an OCA25 chemical contact angle meter and the surface hydrophobicity of the web was characterized by angle.
Antibacterial property test after loading eugenol: and respectively adding 2.5mg/mL eugenol into the prepared fiber solution, and stirring for 1h to prepare the electrostatic spinning solution carrying the antibacterial substance, wherein the spinning process is the same as that of the no-load film. Gram-negative bacteria Escherichia coli and gram-positive bacteria Staphylococcus aureus were selected as subjects. The fibrous membrane was made into a disc 5mm in diameter by a punch and sterilized under an ultraviolet lamp for 30min. 100. Mu.L of the bacterial suspension (1X 106 CFU/mL) is uniformly coated on the sterilized culture medium, then a fiber membrane is attached to the surface of the culture medium, and the culture is carried out for 24 hours in a constant temperature incubator at 37 ℃, and the diameter of a bacteriostasis zone is measured by a vernier caliper.
The test results of the nanofiber membrane performance are shown in table 1, and as can be seen from table 1, the mechanical properties, water blocking performance and antibacterial performance of the nanofiber membrane in the examples are significantly higher than those of the comparative examples.
TABLE 1 comparison of nanofiber membrane performance
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (10)
1. A preparation method of highland barley prolamin is characterized in that highland barley distillers' grains are dried in an electric heating blow-drying box, and dried samples are crushed and sieved; adding the sample powder into ethanol water solution, stirring with a magnetic stirrer, and heating in water bath for 120 min; and centrifuging the solution, adding water into the supernatant, precipitating, centrifuging, collecting the precipitate, and freeze-drying to obtain the target product.
2. The method of claim 1, wherein the sieving is a 40 mesh sieve.
3. The method of claim 1, wherein the aqueous ethanol solution is a 75% aqueous ethanol solution.
4. The method according to claim 1, wherein the water bath heating temperature is 30 to 50 ℃.
5. The method according to claim 1, wherein the centrifugation step is specifically centrifugation at 5000g for 15min.
6. Highland barley prolamin, characterized in that it is prepared by the preparation method of claims 1-5.
7. The prolamin nanofiber membrane is characterized by comprising the following components in parts by weight: 15-20% of zein, 5-10% of highland barley zein, 2-3% of glycerol, 3-7% of cyclodextrin and the balance of acetic acid.
8. The prolamin nanofiber membrane according to claim 7, wherein the highland barley prolamin is highland barley prolamin according to claim 6.
9. The method for preparing an alcohol soluble protein nanofiber membrane according to claim 7, wherein the components are uniformly mixed according to a proportion, and an electrostatic spinning membrane is prepared on an electrostatic spinning machine.
10. The method of claim 9, wherein the electrostatic spinning machine voltage is 17kV and the distance from the needle tip to the collector is maintained at 13cm.
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