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CN109485862A - A kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material - Google Patents

A kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material Download PDF

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CN109485862A
CN109485862A CN201811387485.9A CN201811387485A CN109485862A CN 109485862 A CN109485862 A CN 109485862A CN 201811387485 A CN201811387485 A CN 201811387485A CN 109485862 A CN109485862 A CN 109485862A
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epsilon
polylysine
cellulose
antibacterial material
dialdehyde
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张黎明
李妍
时文佳
何希宏
何志娜
戴玉杰
彭巧玲
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Tianjin University of Science and Technology
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    • A01N43/14Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom

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Abstract

The present invention relates to a kind of dialdehyde celluloses to be grafted epsilon-polylysine antibacterial material, by cellulose oxidation at dialdehyde cellulose, using it as carrier, using graft reaction, according to certain aldehyde radical molar ratio, using epsilon-polylysine modified cellulose, epsilon-polylysine is grafted on dialdehyde microcrystalline cellulose, dialdehyde cellulose epsilon-polylysine antibacterial material, this antibacterial material simple process are prepared with this, it has no toxic side effect, while there is good bacteriostatic activity.Using penicillin as positive control, LB liquid medium is negative control, and the minimum inhibitory concentration (MIC) to Escherichia coli (E.coli), staphylococcus aureus (S.aureus) is 7.5mg/mL;Minimum inhibitory concentration (MIC) to salmonella (S.typhimurium) is 15mg/mL;Minimum inhibitory concentration (MIC) to sarcine (S.lutea) and bacillus subtilis (B.subtilis) is 30mg/mL.Research and development for Novel antibacterial material provide new approaches.

Description

A kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material
The present invention relates to the preparation sides that a kind of dialdehyde cellulose grafting epsilon-polylysine inhibits the antibacterial material of bacterial growth Method.Be grafted with epsilon-polylysine (ε-PL) anti-by certain aldehyde radical molar ratio using the dialdehyde cellulose of certain oxidizability It answers, by increasing positive charge on graft, in conjunction with substance electronegative in bacteria cell wall, and then inhibits bacterial growth, belong to In the innovation area of antibacterial material synthesis.
Background technique
Cellulose (cellulose) is the most abundant natural reproducible polysaccharide of content in nature, is important biomass One of material has the characteristics such as biodegradability, bio-compatibility;The advantages that at low cost, purposes is wide, sustainable development.So And the interaction of self structure and molecule interchain because of cellulose limits its scope of application, such as flexibility is poor, film forming The poor, limited strength of property, not resistant to chemical etching etc., therefore cellulose is modified.For a long time, people utilize various methods pair Cellulose is modified, and to widen its application field, such as cellulose is esterified, is etherified, aoxidizes and is graft-polymerized.Dialdehyde Cellulose (Dialdehyde cellulose, DAC) is obtained with periodic acid or periodate oxidized cellulose, and fiber can be made Two secondary hydroxy oxidations of plain chain element are at aldehyde radical, its reaction vigor greatly improves compared with cellulose.Dialdehyde cellulose molecule Active group in chain, such as amino and aldehyde radical etc. can react with other groups such as amino, and then carry out function to cellulose It can be modified;In addition, dialdehyde cellulose can also prepare new material with other substance reactions such as functional material, bioactive materials. During periodate oxidation, the crystallinity of oxycellulose declines with the raising of degree of oxidation.Through periodate oxidation Treated, and cellulose has good physical mechanical property, not only changes the structure of cellulose, while assigning oxidized fibre The many new functions of element, have expanded the application field of cellulose significantly, have obtained this natural green recyclable materials of cellulose More it is widely applied.
Amino acid and its derivative are the basic units of constitutive protein matter, are widely used in medicine, food, feed, cosmetics The fields such as industry.Amino group in amino acid can occur schiff bases (Schif fbase) with the aldehyde radical of dialdehyde cellulose and react. Schiff bases have unique physical material performance, the physiology such as good Coordinative Chemistry performance and unique antibacterial, anticancer, weeding Activity.In recent years, in medical domain, amino acid and the schiff bases that high molecular material generates have antibacterial, sterilization, antitumor, anti- The bioactivity of virus, and its complex is because with stronger fat-soluble and Cell permeable, so its antimicrobial spectrum is wider, and It is not likely to produce drug resistance, possesses better pharmaceutical value.Thus using amino acid molecular as be grafted bridge, to dialdehyde cellulose into Row graft modification will all have great importance for the development and utilization of new function material.
Epsilon-polylysine (ε-PL) is to be formed by connecting by lysine residue by the amido bond that α-carboxyl and epsilon-amino are formed Homopolymerization polypeptide, scope of restraining fungi is wide, highly-safe, is just applied to food antiseptic early in the eighties.But due to epsilon-polylysine With water-soluble characteristic, application range is greatly limited.It is presented most when the molecular weight of epsilon-polylysine is between 3600-4300 Good bacteriostatic activity can then lose bacteriostatic activity when molecular weight is lower than 1300.And it is not influenced by pH value, to thermostabilization.Research It was found that it can not only inhibit the preferable gram-positive bacteria of heat resistance, moreover it is possible to inhibit the gram-negatives such as Escherichia coli, salmonella Property bacterium, meanwhile, epsilon-polylysine also functions to good fungistatic effect to the growth of saccharomycete, lactobacillus bulgaricus.But to withered The growth inhibitory effect of careless bacillus and aspergillus niger be not it is obvious that carry out combined processing to epsilon-polylysine with acetic acid, can Enhance the inhibiting effect to bacillus subtilis.The antifungal mechanism of epsilon-polylysine is mainly to pass through the cell membrane for destroying microorganism Structure eventually leads to cell death to interrupt the substance of cell, energy and information transmitting.Epsilon-polylysine is cation form Face active material has amino, and positively charged in water, positive charge can be in conjunction with the electronegative site of bacterium surface;Intramolecule There is hydrophobic methylene, there are hydrophilic carboxyl and amino in outside.Utilize epsilon-polylysine excellent bacteriostasis property and amino The characteristic of schiff base reaction occurs with aldehyde radical, novel waterproof antibacterial material is prepared with this.
By cellulose oxidation at dialdehyde cellulose, using it as carrier, using graft reaction, by certain aldehyde radical molar ratio, Using epsilon-polylysine modified cellulose, epsilon-polylysine is grafted on dialdehyde cellulose, dialdehyde cellulose ε-is prepared with this Polylysine antibacterial material, can theoretically increase positive charge on graft, graft by with it is negatively charged in bacteria cell wall Substance combine, to improve its fungistatic effect.In addition, aldehyde radical and amino progress nucleophilic addition obtain seat in reaction process The complex of husband's alkali structure, amino acids schiff bases and its application equally has the uniquenesses such as antibacterial, sterilization, antitumor, antiviral Medicinal effects.
Synthesizing new cellulose amino acid graft is designed, its bacteriostatic activity and other characteristics are carried out comprehensive, deep Research and analysis are all of great significance to the research and development of abundant antibacterial material.
Summary of the invention
It is an object of the invention to synthesize a kind of novel suppression of solid powdery with epsilon-polylysine using dialdehyde cellulose Bacterium material.The method is mainly using positive charge in antibacterial material is increased, by conjunction with substance electronegative in bacteria cell wall, And then inhibit the growth of bacterium.Dialdehyde cellulose is the C of sodium metaperiodate selectively oxycellulose2And C3Position hydroxyl is at aldehyde radical And obtain, graft reaction can occur with the amino in epsilon-polylysine and generate schiff bases for aldehyde radical, and schiff bases also has antibacterial Effect.
The purpose of the present invention is what is be achieved through the following technical solutions, includes the following steps:
A kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material, feature its be to include walking as follows It is rapid:
(1) epsilon-polylysine is dissolved in the deionized water of certain volume, adjusts medium to predetermined pH with NaOH solution, presses Dialdehyde cellulose is added in the molar ratio of aldehyde radical and epsilon-polylysine according to dialdehyde cellulose, is then grafted at a certain temperature It reacts to the scheduled time;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at a certain temperature, obtain the grafting antibacterial material of epsilon-polylysine Material.
The advantages and positive effects of the present invention are:
(1) the invention is characterized in that containing seat by the way that dialdehyde cellulose is added into epsilon-polylysine aqueous solution and produces The compound of husband's alkali structure, by increasing positive charge on graft, to inhibit the growth of bacterium.Resist compared to traditional Raw element class drug, this method is at low cost, high-efficiency environment friendly, easily operated and be widely used.
(2) present invention raw material for being taken in realizing fungistatic effect experiment is cellulose, cellulose have it is cheap, The features such as distribution is wide, structural property is unique.Epsilon-polylysine of the present invention is wide with scope of restraining fungi, safety is non-hazardous, The advantages that being conveniently easy to get, be environment friendly and pollution-free, using extremely wide in all trades and professions.
Detailed description of the invention
The Fourier of the dialdehyde cellulose grafting epsilon-polylysine antibacterial material of Fig. 1 epsilon-polylysine, different aldehyde group contents Infrared spectroscopy (A) epsilon-polylysine;(B) dialdehyde cellulose of different aldehyde group contents is grafted epsilon-polylysine antibacterial material a.5.514mmol/g;b.5.572mmol/g;c.5.981mmol/g;d.6.685mmol/g;e.6.972mmol/g.
Fig. 2 dialdehyde cellulose, epsilon-polylysine, dialdehyde cellulose are grafted the scanning electron microscope of epsilon-polylysine antibacterial material Scheme (A) dialdehyde cellulose;(B) epsilon-polylysine;(C) dialdehyde cellulose is grafted epsilon-polylysine
Bacteriostatic activity (A) the sarcine S.lutea of Fig. 3 dialdehyde cellulose grafting epsilon-polylysine antibacterial material;(B) E. coli;(C) staphylococcus aureus S.aureus;(D) bacillus subtilis B.subtilis;(E) Salmonella Bacterium S.typhimurium;No. 1-No. 8 graft turbid liquid concentrations are respectively 6.00%, 3.00%, 1.50%, 0.75%, 0.38%, 0.19%, 0.09%, 0;No. 9 penicillin solutions (1mg/mL);No. 10 epsilon-polylysine solution (1mg/mL);No. 11 88.7% dialdehyde cellulose (1mg/mL) that aldehyde group content is.
Specific embodiment
With reference to the accompanying drawing in detail narration the embodiment of the present invention, it should be noted that the present embodiment be it is narrative, no It is restrictive, this does not limit the scope of protection of the present invention.
Following experimental procedure is applied in entire embodiment:
Minimum inhibitory concentration (MIC) detection method of dialdehyde cellulose-epsilon-polylysine antibacterial material to different bacterium:
(1) prepared by dialdehyde cellulose and epsilon-polylysine graft suspension: accurately weighing 6.0g different mol ratio example 44mL aseptic deionized water is added in round-bottomed flask in sterilized graft.It is condensed back stirring 1h under 90 DEG C of water-baths, is made The graft suspension that concentration is 12%.
(2) picking indicator bacteria single colonie is inoculated into 20mL LB culture medium, and 37 DEG C, 220r/min cultivates about 20h.
(3) instruction bacteria culture fluid is corrected to OD with 0.9% physiological saline625=0.1, at this time bacterium amount be about 1~2 × 108CFU/mL.The instruction bacteria culture fluid for taking 100 μ L to proofread be added in 2.9mL LB culture medium be made bacteria suspension it is spare, this When, the concentration of bacteria suspension is 5 × 106CFU/mL。
(4) 11 sterile test tubes are taken to be arranged in a row, every pipe adds 5mL sterilizing LB liquid medium, and taking 5mL concentration is 12% Graft suspension is added the 1st test tube and mixes.Then it therefrom draws 5mL and adds to the 2nd pipe, pressure-vaccum is mixed repeatedly using liquid-transfering gun 5mL is drawn after even again, the 3rd pipe is added.Repeat the above steps successively serial dilution to the 7th pipe, and from the 7th pipe draw 5mL abandon It removes.8th pipe is set as the negative control group without graft, and 5mL culture medium and 5mL physiological saline are added thereto, uses liquid-transfering gun Pressure-vaccum discards 5mL after mixing repeatedly.9th test tube is set as plus the positive control of penicillin (1mg/mL), and 5mL training is added thereto Base and 5mL penicillin are supported, discards 5mL after pressure-vaccum mixes repeatedly with liquid-transfering gun.10th test tube is set as plus epsilon-polylysine (1mg/ ML the epsilon-polylysine solution of 5mL culture medium and 5mL is added in control) thereto, is discarded after pressure-vaccum mixes repeatedly with liquid-transfering gun 5mL.11st test tube be set as plus aldehyde group content be 6.685mmol/g dialdehyde cellulose (1mg/mL) control, thereto plus Enter 5mL culture medium and 5mL dialdehyde cellulose suspension, discards 5mL after pressure-vaccum mixes repeatedly with liquid-transfering gun.
(5) 0.1mL bacteria suspension is added to 11 test tubes respectively, graft suspension is dense in the 1st to the 8th test tube at this time Degree is respectively 6.000%, 3.000%, 1.500%, 0.750%, 0.375%, 0.188%, 0.094%, 0%, every pipe bacterium solution Concentration is about 5 × 105CFU/mL.9th test tube is positive control.
(6) inoculated each test tube is placed in 37 DEG C of shaking tables and 24-30h is cultivated with 220r/min.
(7) test tube is stood into 5min, takes supernatant liquor to test the ultraviolet absorptivity under 600nm, and returned to zero with deionized water. Five kinds of bacteriums are all made of this method and carry out bacteriostatic experiment.
As seen from Figure 1, in 3436cm-1、2900cm-1、1639cm-1Left and right many places peak dies down, these phenomenons show double Aldehyde cellulose and epsilon-polylysine occur graft reaction and generate schiff bases, and the stability of graft is enhanced;Fig. 2 can be seen Out, dialdehyde cellulose, epsilon-polylysine, dialdehyde cellulose/ε-PL graft particle size are different.The particle of dialdehyde cellulose It is larger, size is relatively long, and rough gauffer, illustrate that sodium metaperiodate has the structure of cellulose and corrode and removing Effect;The particle surface of epsilon-polylysine is relatively smooth, no striped gauffer;Dialdehyde cellulose/ε-PL graft particle compared with Particle is smaller for the two, and more mellow and fuller full, surface is also more rougher, this is because the poly- bad ammonia of the cellulose and ε-after oxidation Caused by graft reaction occurs for acid.From figure 3, it can be seen that dialdehyde cellulose/ε-PL graft antibacterial material has five kinds of bacteriums Obvious fungistatic effect.
The present invention will be further described with reference to the examples below:
Embodiment 1:
(1) epsilon-polylysine is dissolved in 100mL deionized water, is 8.0 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.1, then in 30 DEG C of progress graft reactions 8h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 37 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to sarcine;
Aldehyde group content is dialdehyde cellulose/ε-PL antibacterial material pair that the dialdehyde cellulose of 5.514mmol/g is prepared The minimum inhibitory concentration (MIC) of sarcine is 30mg/mL.
Embodiment 2:
(1) epsilon-polylysine is dissolved in 100mL deionized water, is 8.5 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.1, then in 30 DEG C of progress graft reactions 8h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 37 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to Escherichia coli;
Aldehyde group content is dialdehyde cellulose/ε-PL antibacterial material pair that the dialdehyde cellulose of 5.514mmol/g is prepared The minimum inhibitory concentration (MIC) of Escherichia coli is 7.5mg/mL.
Embodiment 3:
(1) epsilon-polylysine is dissolved in 100mL deionized water, is 8.5 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.2, then in 30 DEG C of progress graft reactions 8h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 47 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to staphylococcus aureus;
Aldehyde group content is dialdehyde cellulose/ε-PL antibacterial material pair that the dialdehyde cellulose of 5.514mmol/g is prepared The minimum inhibitory concentration (MIC) of staphylococcus aureus is 7.5mg/mL.
Embodiment 4:
(1) epsilon-polylysine is dissolved in 110mL deionized water, is 8.7 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.1, then in 30 DEG C of progress graft reactions 8h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 37 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to bacillus subtilis;
Aldehyde group content is dialdehyde cellulose/ε-PL antibacterial material pair that the dialdehyde cellulose of 5.514mmol/g is prepared The minimum inhibitory concentration (MIC) of bacillus subtilis is 30mg/mL.
Embodiment 5:
(1) epsilon-polylysine is dissolved in 110mL deionized water, is 9.0 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.3, then in 40 DEG C of progress graft reactions 8h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 50 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to salmonella;
Aldehyde group content is dialdehyde cellulose/ε-PL antibacterial material pair that the dialdehyde cellulose of 5.514mmol/g is prepared The minimum inhibitory concentration (MIC) of salmonella is 15mg/mL.
Embodiment 6:
(1) epsilon-polylysine is dissolved in 110mL deionized water, is 9.0 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.3, then in 40 DEG C of progress graft reactions 8h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 58 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to sarcine;
Aldehyde group content is dialdehyde cellulose/antibacterial material of ε-PL that the dialdehyde microcrystalline cellulose of 6.725mmol/g is prepared Expect that the minimum inhibitory concentration (MIC) of sarcine be 30mg/mL.
Embodiment 7:
(1) epsilon-polylysine is dissolved in 120mL deionized water, is 8.5 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.3, then in 40 DEG C of progress graft reactions 7h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 56 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to Escherichia coli;
Aldehyde group content is dialdehyde cellulose/antibacterial material of ε-PL that the dialdehyde microcrystalline cellulose of 6.725mmol/g is prepared Expect that the minimum inhibitory concentration (MIC) of Escherichia coli be 7.5mg/mL.
Embodiment 8:
(1) epsilon-polylysine is dissolved in 100mL deionized water, is 9.0 with NaOH solution adjusting medium to pH, by dialdehyde Dialdehyde cellulose is added in the aldehyde radical of cellulose and the molar ratio of epsilon-polylysine 1: 0.2, then in 30 DEG C of progress graft reaction 8h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 40 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to staphylococcus aureus;
Aldehyde group content is dialdehyde cellulose/antibacterial material of ε-PL that the dialdehyde microcrystalline cellulose of 6.725mmol/g is prepared Expect that the minimum inhibitory concentration (MIC) of staphylococcus aureus be 7.5mg/mL.
Embodiment 9:
(1) epsilon-polylysine is dissolved in 110mL deionized water, is 9.0 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.2, then in 40 DEG C of progress graft reactions 6h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 58 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to bacillus subtilis;
Aldehyde group content is dialdehyde cellulose/antibacterial material of ε-PL that the dialdehyde microcrystalline cellulose of 6.725mmol/g is prepared Expect that the minimum inhibitory concentration (MIC) of bacillus subtilis be 30mg/mL.
Embodiment 10:
(1) epsilon-polylysine is dissolved in 110mL deionized water, is 8.5 with NaOH solution adjusting medium to pH, according to double Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine 1: 0.3, then in 30 DEG C of progress graft reactions 6h;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, will Gained graft naturally dry, grinding uniformly, then are dried in vacuo at 48 DEG C, obtain grafting epsilon-polylysine antibacterial material.
(3) antibacterial material is subjected to bacteriostatic experiment to salmonella;
Aldehyde group content is dialdehyde cellulose/antibacterial material of ε-PL that the dialdehyde microcrystalline cellulose of 6.725mmol/g is prepared Expect that the minimum inhibitory concentration (MIC) of salmonella be 15mg/mL.

Claims (4)

1. a kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material, feature its be to include walking as follows It is rapid:
(1) epsilon-polylysine is dissolved in the deionized water of certain volume, adjusts medium to predetermined pH, according to double with NaOH solution Dialdehyde cellulose is added in the aldehyde radical of aldehyde cellulose and the molar ratio of epsilon-polylysine, then carries out graft reaction at a certain temperature To the scheduled time;
(2) it after reactor is cooled to room temperature, filters and removes filtrate, filter cake successively uses deionized water and ethanol washing, by gained Graft naturally dry, grinding uniformly, then are dried in vacuo at a certain temperature, obtain grafting epsilon-polylysine antibacterial material.
2. a kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material, feature its be that step (1) is described The deionized water volume of addition is 100mL-120mL, and the pH value range of aqueous solution is 8.0-9.0, and dialdehyde cellulose and ε-are poly- The aldehyde radical molar ratio of lysine be 1: 0.1-1: 0.3,30 DEG C -40 DEG C of reaction temperature, reaction time 6h-8h.
3. a kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material, feature its be that step (2) is described Medium successively uses deionized water and ethanol washing 2-3 times, is dried in vacuo in 37 DEG C of -58 DEG C of temperature ranges.
4. a kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material, feature its be obtained by step (2) Dialdehyde cellulose be grafted epsilon-polylysine antibacterial material to bacterium for example staphylococcus aureus, Escherichia coli, bacillus subtilis, Salmonella, sarcine have apparent bacteriostatic activity.
CN201811387485.9A 2018-11-21 2018-11-21 A kind of preparation method of dialdehyde cellulose grafting epsilon-polylysine antibacterial material Pending CN109485862A (en)

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CN111499928A (en) * 2019-12-30 2020-08-07 天津科技大学 Method for preparing cellulose antibacterial material by using polylysine as cross-linking agent
CN111974367A (en) * 2020-09-03 2020-11-24 天津科技大学 Preparation method of polylysine modified cellulose material for adsorbing copper ions
CN112426377A (en) * 2020-10-27 2021-03-02 浙江理工大学 Water-soluble antibacterial spray and application thereof
CN112851951A (en) * 2021-01-14 2021-05-28 中国科学院理化技术研究所 Dialdehyde chitosan grafted with epsilon-polylysine and preparation method and application thereof
CN113768949A (en) * 2021-10-08 2021-12-10 徐州医科大学 Application of epsilon-polylysine or hydrochloride thereof in preparation of medicine for inhibiting Cronobacter sakazakii or intervening Cronobacter sakazakii biofilm
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CN113768949A (en) * 2021-10-08 2021-12-10 徐州医科大学 Application of epsilon-polylysine or hydrochloride thereof in preparation of medicine for inhibiting Cronobacter sakazakii or intervening Cronobacter sakazakii biofilm
CN115178029A (en) * 2022-06-20 2022-10-14 苏州大学 Air filtering membrane and preparation method and application thereof
CN115178029B (en) * 2022-06-20 2024-08-09 南京威盾新能源科技有限公司 Air filtering membrane and preparation method and application thereof
CN116158994A (en) * 2023-02-27 2023-05-26 天津科技大学 Caries preventing toothpaste containing 2,3-dialdehyde microcrystalline cellulose and preparation method thereof

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