CN113151931B

CN113151931B - Method for improving tensile strength of gellan gum-polylysine fiber and application thereof

Info

Publication number: CN113151931B
Application number: CN202110441106.5A
Authority: CN
Inventors: 吴剑荣; 张颖; 郭钰; 俞科静; 胡锦华; 詹晓北
Original assignee: Jiangnan University
Current assignee: Jiangnan University
Priority date: 2021-04-23
Filing date: 2021-04-23
Publication date: 2022-03-25
Anticipated expiration: 2041-04-23
Also published as: CN113151931A

Abstract

The invention discloses a method for improving the tensile strength of gellan gum-polylysine fibers and application thereof, belonging to the field of biological materials. According to the invention, several carbohydrate and protein substances containing heat are added into the gellan gum-polylysine spinning system, so that the tensile strength of the fiber is enhanced; then embedding lipid substances and stanching and promoting healing substances into the liposome and attaching the liposome to the fibers woven into blocks, thereby preparing the multifunctional fibers with higher tensile strength. Carbohydrate, protein and lipid substances are added into the gellan gum-polylysine fiber preparation system, so that the tensile strength of the fiber is improved, and the fiber contains certain caloric substances and blood coagulation factors. The fiber material has multiple functions, and can be applied to dressings, operation lines and outdoor field emergency equipment.

Description

Method for improving tensile strength of gellan gum-polylysine fiber and application thereof

Technical Field

The invention relates to a method for improving the tensile strength of gellan gum-polylysine fibers and application thereof, belonging to the field of biological materials.

Background

With the large-scale development of food industry in China, the gellan gum becomes a novel food additive, thickener and preservative with lower dosage, better effect and more complete functions by virtue of the unique advantages of the gellan gum, and is widely used. Polylysine (PLL) is a natural preservative, the chemical composition of which is polypeptide composed of L-Lysine, and the polypeptide can be changed into single Lysine after being digested to become a nutrition enhancer for human body, and the polylysine has the characteristics of no toxic and side effects and high safety.

The polyionic complex is formed by reacting a polyelectrolyte with an oppositely charged polyelectrolyte in an aqueous solution. The epsilon-polylysine is rich in cations, generates stronger electrostatic acting force with substances with anions and has good penetrating power on biological membranes. Gellan gum, when heated in the presence of cations, cools to form a gel. In addition, gellan gum and polylysine can be used to produce relatively uniform fibers by in situ polymerization and wet spinning processes. By using a simple wet spinning machine (wet spinning), gellan gum aqueous solution with a certain concentration can be uniformly propelled into stationary liquid polylysine solution through a uniform-speed propulsion pump, and fiber threads fully reflected are timely drawn by using a uniform-speed reeling machine at the other end of a fixed domain.

Gellan gum has unique rheological properties and is a good carrier material for active compounds. It has been reported that gellan gum and nano titanium dioxide can form wound healing biomembranes after being compounded, and it is also pointed out that titanium oxide nanotubes can be mixed with gellan gum to obtain a gellan titanium nanotube-based material which has good antibacterial activity, biocompatibility and acceptable mechanical strength. Amaike et al found that gellan gum can form polyion complex hydrogels with polylysine in aqueous solution and utilize droplets of this gellan gum-polylysine complex to form fibers under the influence of gravity. However, the fibers obtained are not sufficient, and the mechanical properties of these hydrogel fibers are still to be improved. Further studies have shown the potential of this fiber for use as a surgical suture, which also suggests its potential for use in the pharmaceutical industry. Therefore, it is necessary to develop gellan gum-polylysine fiber with higher mechanical strength and suitable for the pharmaceutical industry (such as having hemostatic and healing promoting effects).

Disclosure of Invention

[ problem ] to provide a method for producing a semiconductor device

The technical problems to be solved in practice by the invention are as follows: provides a method for preparing gellan gum-polylysine fiber with higher mechanical strength.

[ technical solution ] A

The invention aims to overcome the limitations and the defects of the prior art and provides a method for preparing gellan gum-polylysine fiber with higher tensile strength, and the fiber also contains caloric substances and blood coagulation factors. According to the invention, saccharides and protein substances with heat are added into a spinning system, and water-insoluble nutrient substances and blood coagulation factors are attached and embedded on the surface of the fiber, so that the tensile strength and spinnability of the fiber are improved, and the fiber has the effects of high heat, hemostasis and healing promotion, and can be used as an operation line, a dressing and outdoor field equipment. Through a series of optimization improvements, the preparation of the gellan gum-polylysine fiber with higher tensile strength is finally realized.

The first purpose of the invention is to provide a method for improving the mechanical property of gellan gum-polylysine fiber, which is to add nutrient substances into spinning solution, wherein the nutrient substances comprise saccharides and/or proteins, and the addition amount of the nutrient substances in the spinning solution is 0.1-7.5% w/v.

Preferably, the addition amount of the nutrient in the spinning solution is 0.1-3.5% w/v.

In one embodiment of the invention, the sugar comprises glucose or maltose.

Preferably, the amount of sugar added to the spinning dope is 0.1% to 1.0% w/v.

In one embodiment of the invention, the protein comprises one or more of a soy peptide and a fish collagen peptide.

Preferably, the addition amount of the protein in the spinning solution is 0.1-3.0% w/v; more preferably, the amount of protein added to the spinning solution is from 0.1% to 0.75% w/v.

Preferably, the addition amount of the soybean peptide is 0.1-1.0% w/v, and the addition amount of the fish collagen peptide is 0.5-2.0% w/v.

In one embodiment of the present invention, when the nutrients are saccharides and proteins, the mass ratio of the saccharides to the proteins is (1-5) to (1-5).

Preferably, the addition amount of the nutrient substances in the spinning solution is 0.5-1.5% w/v of glucose, 0.1-1.0% w/v of soybean peptide and 0.5-2.0% w/v of fish collagen peptide.

The second purpose of the invention is to provide a method for preparing the gellan gum-polylysine fiber, wherein the gellan gum-polylysine fiber is prepared by wet spinning, and a spinning system comprises gellan gum, polylysine and nutrient substances; the nutrients comprise sugars and/or proteins; the addition amount of the nutrient substances in the spinning solution is 0.1-7.5% w/v.

In one embodiment of the invention, the mass ratio of gellan gum, polylysine and nutrients is (1-4): (2-10): (1-15).

In one embodiment of the invention, the sugar comprises glucose or maltose.

Preferably, the amount of sugar added to the spinning solution is 0.1% to 1.0%.

Preferably, the addition amount of the protein in the spinning solution is 0.1-3.0%; more preferably, the amount of protein added to the spinning solution is 0.1% to 0.75%.

Preferably, the addition amount of the nutrients in the spinning solution is 0.5% w/v fish collagen peptide, 1.0% w/v glucose and 0.5% w/v soybean peptide.

In one embodiment of the invention, the spinning system comprises the following raw materials in parts by weight (w/v): 0.5 to 2.0 percent of gellan gum, 0.5 to 1.5 percent of glucose, 0.1 to 1.0 percent of soybean peptide, 0.5 to 2.0 percent of fish collagen peptide and 1.0 to 5.0 percent of polylysine; the liposome system comprises the following raw materials in parts by weight (in an organic phase): 1 to 3 percent of lecithin, 0.25 to 1 percent of cholesterol, 100 to 900 percent of deionized water, 0.1 to 0.3 percent of ginsenoside, 0.1 to 3 percent of thymol and 0.1 to 1.0 percent of vitamin. Wherein, the glucose and the soybean peptide can not only supplement nutrition but also improve the tensile strength of the fiber through the interaction with the gellan gum; the fish collagen peptide has the function of promoting wound healing and improving the tensile strength of the fiber through the interaction with gellan gum; lipids act to improve the mechanical properties of the fiber and to supplement the fiber with lipid nutrients.

In one embodiment of the invention, the spinning system comprises the following raw materials in parts by weight (w/v): gellan gum 1.0% (low acyl gellan gum: high acyl gellan gum 5:1), glucose 1.0%, soybean peptide 0.5%, and polylysine 5.0%.

In one embodiment of the invention, the spinning stock solution is discharged from a spinning nozzle at a temperature of 60-90 ℃ in the spinning process, the pumping speed of a fixed bath at a temperature of 40-80 ℃ is 0.1-1.0 mL/min, and the drawing speed is 20-50 cm/min.

In one embodiment of the invention, the oil-water ratio in the liposome preparation process is 1: 1-1: 9, the mass ratio of phospholipid to ginsenoside is 1:0.5, the phenol-lipid ratio of thymol is 1-2 mg/mL, and the vitamin k loading is about 20%.

In one embodiment of the invention, the method comprises the steps of:

(1) preparation of spinning stationary liquid: weighing polylysine according to the weight part, dissolving the polylysine in ultrapure water, stirring the solution by using a glass rod until the solution is clear, and pouring the solution into a fixed liquid tank.

(2) Preparing a spinning solution: weighing a certain weight part of high-acyl gellan gum, low-acyl gellan gum, glucose, soybean peptide and fish collagen peptide, dissolving in a certain amount of ultrapure water, storing in a 10mL syringe after completely dissolving, and heating to 60 ℃ for later use.

(3) The injector is arranged on the propeller, the needle head is inserted into the injector, the other end of the needle head is fixed in the polylysine fixing liquid, the injector is propelled at a constant speed, the spinning solution enters the fixing liquid to form fibers, and then the fibers are quickly drawn to a uniform-speed reel to be collected, wherein each 20 fibers are one strand.

(4) Preparing liposome: respectively weighing a certain amount of lecithin, cholesterol, ginsenoside, thymol and vitamin k, dissolving in a proper amount of absolute ethyl alcohol, pouring a certain amount of Phosphate Buffer Solution (PBS) into a beaker, putting into a rotor, slowly injecting an oil phase into the PBS by using an injector under magnetic stirring at the water bath temperature of 50 ℃, continuously stirring for 30min, and stopping heating and stirring until the formed solution has no organic solvent taste after titration is finished.

(5) The fibers from (3) were then woven into 5 x 5 fabric, and the liposome solution (about 500 microliters) was sprayed evenly onto the fabric using a small spray can and allowed to dry at room temperature.

The third purpose of the invention is to provide a gellan gum-polylysine fiber prepared by the method.

The fourth purpose of the invention is to provide the application of the gellan gum-polylysine fiber in textile yarns, medical dressings, surgical sutures, medical and aesthetic products, food packaging, outdoor field emergency equipment and the like.

In one embodiment of the present invention, the gellan gum-polylysine fiber has high calories and can be used as an energy supplement for medical personnel in an emergency to rapidly replenish energy.

Has the advantages that:

the invention optimizes the gellan gum-polylysine fiber preparation system reported at present, adds carbohydrate, protein and lipid substances, improves the tensile strength of the fiber, improves the breaking strength from 0.33cN/dtex to 0.71cN/dtex, improves 115.15%, and simultaneously endows the fiber with the characteristic of high heat; and substances for promoting healing and blood coagulation factors are attached to the surface of the fiber, so that the fiber has the effect of stopping bleeding, and finally the multifunction of the gellan gum-polylysine fiber is realized.

Drawings

FIG. 1 is an appearance diagram of gellan gum-polylysine fiber containing clotting factors.

Detailed Description

The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.

Gellan gum is available from CP Kelco corporation, usa; polylysine was purchased from fresh Yinhong bioengineering, Inc., Zhejiang; the small molecular soybean peptide powder is purchased from Saint Jiade Biotech limited of Qufukang; ginsenoside was purchased from Xian Siji Biotech Co., Ltd; the rest reagents are purchased from chemical reagents of national medicine group, Inc.; the propeller is purchased from pump industry Co., Ltd, Shenchen, assigned to City; ultra-low speed collection drums (0.1-300RPM) were purchased from sbeining electrospinning equipment; the YG020A type electronic single yarn strength tester is purchased from Shanghai precision scientific instruments; the heat collection type constant temperature magnetic stirring bath is purchased from Zhengzhou great wall science and trade Co.

Test method for breaking strength: the breaking strength and elongation at break of the fibers were determined with reference to GB/T4743-1995.

Example 1: method for improving gellan gum-polylysine high fiber tensile strength by adopting glucose

A method for improving the tensile strength of gellan gum-polylysine fibers comprises the following steps:

(1) preparation of spinning stationary liquid: 2.5g of polylysine was weighed out and dissolved in 50mL of ultrapure water, stirred with a glass rod until the solution was clear and poured into a fixed liquid bath.

(2) Preparing a spinning solution: 0.0417g of high acyl gellan gum, 0.2083g of low acyl gellan gum and 0.25g of glucose (1%) were weighed and dissolved in 25mL of ultrapure water, and after complete dissolution, they were stored in a 10mL syringe and heated to 60 ℃ for use.

(3) The injector (60 ℃) is arranged on a propeller, the needle head is inserted into the injector, the other end of the needle head is fixed in polylysine stationary liquid (40 ℃), the injector is propelled at the speed of 0.5mL/min, the spinning solution enters the stationary liquid to form fibers, and then the fibers are rapidly pulled to a 40cm/min constant-speed reel to be collected, and each 20 fibers are one strand.

Referring to the breaking strength of the gellan gum-polylysine fiber prepared by the method of this example using 0.5% glucose, 1.0% glucose and 1.5% glucose, respectively, as shown in table 1, it can be seen that the tensile strength of the gellan gum-polylysine fiber can be improved by adding glucose, the spinning condition is better, and preferably, the breaking strength and the breaking elongation are combined, and the addition amount of glucose is 1.0%.

TABLE 1

Example 2: method for improving gellan gum-polylysine high fiber tensile strength by adopting maltose

A method for improving the tensile strength of gellan gum-polylysine high fibers comprises the following steps:

(2) Preparing a spinning solution: 0.0417g of high acyl gellan gum, 0.2083g of low acyl gellan gum and 0.25g of maltose (1%) were weighed and dissolved in 25mL of ultrapure water, and after complete dissolution, they were stored in a 10mL syringe and heated to 60 ℃ for use.

Referring to the method of the present example, the breaking strength of the gellan gum-polylysine fiber prepared by using 0.5% maltose, 1.0% maltose and 1.5% maltose is shown in table 2, and it can be seen that the addition of maltose can improve the tensile strength of the gellan gum-polylysine fiber, and the spinning condition is better.

TABLE 2

Example 3: method for improving gellan gum-polylysine high fiber tensile strength by adopting protein

(2) Preparing a spinning solution: 0.0417g of high acyl gellan gum, 0.2083g of low acyl gellan gum and 0.125g of soybean peptide were weighed, dissolved in 25mL of ultrapure water, and after complete dissolution, they were stored in a 10mL syringe and heated to 60 ℃ for use.

TABLE 3

Example 4: method for improving gellan gum-polylysine fiber tensile strength by adopting saccharides and proteins

(2) Preparing a spinning solution: 0.0417g of high acyl gellan gum, 0.2083g of low acyl gellan gum, 0.25g of glucose and 0.125g of soybean peptide protoprotein peptide were weighed, dissolved in 25mL of ultrapure water, and after complete dissolution, stored in a 10mL syringe, and heated to 60 ℃ for use.

As can be seen from Table 4, the gellan gum-polylysine fibers obtained by adding 1.0% glucose alone had a breaking strength of 0.34cN/dtex, which was only increased by 0.01 cN/dtex; the breaking strength of the gellan gum-polylysine fiber obtained by independently adding 0.5 percent of soybean peptide is 0.41cN/dtex, which is only improved by 0.08 cN/dtex; and the combined use of glucose and soybean peptide results in a gellan gum-polylysine fiber with a breaking strength of 0.55cN/dtex, an increase of 0.22cN/dtex, and a breaking strength increase rate of up to 67%, indicating that glucose and protein have synergistic effect in increasing the breaking strength of gellan gum-polylysine fiber.

TABLE 4

Example 5:

(2) Preparing a spinning solution: 0.0417g of high acyl gellan gum, 0.2083g of low acyl gellan gum, 0.25g of glucose, 0.125g of soybean peptide and 0.125g of fish collagen peptide were weighed, dissolved in 25mL of ultrapure water, and after complete dissolution, stored in a 10mL syringe, heated to 60 ℃ for use.

The gellan gum-polylysine fiber prepared by the embodiment has the breaking strength of 0.71cN/dtex, the elongation at break of 8.0%, and the spinning condition is better.

Example 6:

(2) Preparing a spinning solution: 0.0417g of high acyl gellan gum, 0.2083g of low acyl gellan gum, 0.25g of glucose, 0.125g of soybean peptide and 0.75g of fish collagen peptide were weighed, dissolved in 25mL of ultrapure water, and after complete dissolution, stored in a 10mL syringe, heated to 60 ℃ for use.

(4) Preparing liposome: 0.4g of lecithin, 0.1g of cholesterol, 0.2g of ginsenoside, 0.14g of thymol and 0.02g of vitamin k are respectively weighed and dissolved in 20mL of absolute ethyl alcohol, 20mL of Phosphate Buffer Solution (PBS) is poured into a beaker, a rotor is placed, the oil phase is slowly injected into the PBS by using an injector under the magnetic stirring at the water bath temperature of 50 ℃, the stirring is continued for 30min, and the heating and the stirring are stopped until the formed solution has no organic solvent taste after the titration is finished.

The gellan gum-polylysine fiber prepared by the embodiment has the breaking strength of 0.51cN/dtex, the elongation at break of 3.3 percent, good spinning effect and easy breakage.

Example 7:

(2) Preparing a spinning solution: 0.0417g of high acyl gellan gum, 0.2083g of low acyl gellan gum, 0.25g of glucose, 0.125g of soybean peptide and 0.5g of fish collagen peptide were weighed, dissolved in 25mL of ultrapure water, and after complete dissolution, stored in a 10mL syringe, heated to 60 ℃ for use.

(4) Preparing liposome: 0.4g of lecithin, 0.067g of cholesterol, 0.2g of ginsenoside, 0.14g of thymol and 0.02g of vitamin k are respectively weighed and dissolved in 20mL of absolute ethyl alcohol, 180mL of Phosphate Buffer Solution (PBS) is poured into a beaker, a rotor is placed, the oil phase is slowly injected into the PBS by a syringe under magnetic stirring at the water bath temperature of 50 ℃, the stirring is continued for 30min, and after the titration is finished, the heating and the stirring are stopped until the formed solution has no organic solvent taste.

The gellan gum-polylysine fiber prepared by the embodiment has the breaking strength of 0.47cN/dtex, the elongation at break of 2.0 percent, good spinning condition and difficult breakage.

TABLE 5

Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims

1. A method for improving the mechanical property of gellan gum-polylysine fibers is characterized in that nutrients are added into spinning solution, the nutrients comprise saccharides and/or proteins, and the addition amount of the nutrients in the spinning solution is 0.1-7.5% w/v; the saccharide comprises glucose or maltose; the protein includes one or more of a soybean peptide and a collagen peptide.

2. The method of claim 1, wherein when the nutrients are saccharides and proteins, the mass ratio of saccharides to proteins is (1-5) to (1-5).

3. The process of claim 1, wherein the amount of sugar added to the dope is 0.1% to 1.0% w/v.

4. The process of claim 1, wherein the protein is added to the dope in an amount of 0.1% to 3.0% w/v.

5. The method for preparing the gellan gum-polylysine fiber is characterized in that the gellan gum-polylysine fiber is prepared by wet spinning, and a spinning system comprises gellan gum, polylysine and nutrient substances; the nutrients comprise sugars and/or proteins; the addition amount of nutrient substances in the spinning solution is 0.1-7.5% w/v; the saccharide comprises glucose or maltose; the protein includes one or more of a soybean peptide and a collagen peptide.

6. The method of claim 5, wherein the mass ratio of gellan gum, polylysine and nutrients is (1-4): (2-10): (1-15).

7. The method according to claim 5 or 6, wherein when the nutrients are saccharides and proteins, the mass ratio of the saccharides to the proteins is (1-5) to (1-5).

8. The process according to claim 5, wherein the amount of sugar added to the spinning dope is 0.1% to 1.0% w/v.

9. The process of claim 5, wherein the protein is added to the dope in an amount of 0.1% to 3.0% w/v.

10. Gellan gum-polylysine fibres prepared by the process according to any one of claims 5 to 9.

11. Use of gellan gum-polylysine fiber according to claim 10 in textile threads, medical dressings, surgical sutures, medical and aesthetic, food packaging, outdoor field emergency equipment.