CN108395705A - A kind of edibility antimicrobial preservative film and its preparation method and application - Google Patents

A kind of edibility antimicrobial preservative film and its preparation method and application Download PDF

Info

Publication number
CN108395705A
CN108395705A CN201810054727.6A CN201810054727A CN108395705A CN 108395705 A CN108395705 A CN 108395705A CN 201810054727 A CN201810054727 A CN 201810054727A CN 108395705 A CN108395705 A CN 108395705A
Authority
CN
China
Prior art keywords
antimicrobial preservative
preservative film
edibility
mdc
film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201810054727.6A
Other languages
Chinese (zh)
Other versions
CN108395705B (en
Inventor
卢雪梅
张伦
桂水清
刘阿龙
陈朝霞
唐亚男
金小宝
朱家勇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Digital Entropy Dimension Medical Information Technology Co ltd
Original Assignee
Guangdong Pharmaceutical University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangdong Pharmaceutical University filed Critical Guangdong Pharmaceutical University
Priority to CN201810054727.6A priority Critical patent/CN108395705B/en
Publication of CN108395705A publication Critical patent/CN108395705A/en
Application granted granted Critical
Publication of CN108395705B publication Critical patent/CN108395705B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2389/00—Characterised by the use of proteins; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2471/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/05—Alcohols; Metal alcoholates
    • C08K5/053—Polyhydroxylic alcohols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C08K5/175—Amines; Quaternary ammonium compounds containing COOH-groups; Esters or salts thereof

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The present invention relates to a kind of edibility antimicrobial preservative film and its preparation method and application, which is prepared from the following materials：Film forming agent, glycerine, antibacterial peptide MDC, tea polyphenols, Tween 80 and purified water.The film forming agent is gelatine derivative, is prepared from the following materials：Fishskin gelatin, epoxidized soybean oil, sugar ester, Geniposide and purified water.Antimicrobial preservative film of the present invention is using gelatine derivative as film forming agent, with preferable filming performance and mechanical performance, further add the antipathogenic composition being used in compounding with antibacterial peptide MDC and tea polyphenols, with significant anti-bacterial refreshing effect, the raw material of use is that green is edible, it is at low cost, securely and reliably, it can be widely used for the fields such as food fresh keeping, food packaging and tableware packaging.

Description

A kind of edibility antimicrobial preservative film and its preparation method and application
Technical field
This patent belongs to packaging material for food field, and in particular to a kind of edibility antimicrobial preservative film and preparation method thereof and Using.
Background technology
Food-safety problem has become the hot spot of global concern.People are no longer confined to the performance requirement of packaging material for food It is whether degradable, it is more desirable to that there is higher safety and preferable anti-bacterial refreshing effect, to avoid packaging material to food The secondary pollution problem brought.There are three types of current preservative films the most widely used on the market：Polyethylene (PE) film, polyvinyl chloride (PVC) film and polyvinylidene chloride (PVDC) film, although this three classes preservative film has certain fresh-keeping function, they are not Have biodegradability and antibiotic property, some materials may discharge harmful under certain media environment and temperature condition Object causes health potentially hazardous.Therefore, find nontoxic, safety and environmental friendliness alternative materials be at present there is an urgent need for It solves the problems, such as.
Currently, the biodegradabilities such as chitosan, gelatin, starch and the preferable substance of biocompatibility are in packaging material The existing application of industry, these substances derive from a wealth of sources, cheap, environmentally protective, to be increasingly becoming the main of food-grade preservative film Filmogen, however there are still some shortcomings, such as：Chitosan film toughness is poor, gelatin film and starch film hygroscopicity are strong, water preventing ability Difference is not enough to inhibit the growth and breeding of microorganism in addition, the preservative film that the above substance is formed only has weaker antibiotic property, It is difficult to ensure the quality of food.Therefore, existing technology often adds a certain amount of antiseptic in the preparation of preservative film, to obtain Obtain the preferable composite membrane of comprehensive performance." a kind of novel edibility is anti-for the Chinese patent application of 106750580 A of Publication No. CN Bacterium food package film and preparation method thereof " using chitosan, acetic acid solution, gelatin, glycerine, Tween-80 and cinnamon essential oil as raw material, Edibility antibacterial food packaging film obtained has good tensile strength and ductility, and to Escherichia coli, golden yellow Portugal The inhibition of grape coccus is significantly higher than PE preservative films.However, the invention using cinnamon essential oil as antiseptic, has effumability Defect, it is difficult to ensure the long-time stability of preservative film.
The appearance of antibacterial peptide in recent years is that the research of antimicrobial preservative film brings new thinking.Antibacterial peptide (Antimicrobial peptides, AMP) is a kind of resist extraneous pathogenic infection small point that Immune System generates Sub- polypeptide is widely present in insect, plant, animal and human body.Antibacterial peptide Musca domestica cecropin (MDC) are The areas the ORF overall length of a kind of insect antimicrobial peptide of this seminar clone, the gene is 192bp, the precursor of 63 amino acid of codified Albumen, 1~23 amino acids are to guard the signal peptide of 4 peptides ending, and mature peptide contains 40 amino acid, our preliminary in vitro Experimental study shows that antibacterial peptide MDC does not have toxicity, acute subacute safety to human red blood cells, Mice red cell, cultured cell in vitro Property evaluation experimental result also show antibacterial peptide MDC administration after, mouse general status is good, has no that overt toxicity reacts, and toxicity is real 1 animal dead of middle nothing is tested, does not measure median lethal dose.As a kind of antiseptic of safety and environmental protection, antibacterial peptide MDC can effectively press down System includes escherichia coli (E.coli), salmonella (S.paratyphi-B), shigella dysenteriae (S.dysenteriae), a variety of breedings for causing food spoilage microorganism including staphylococcus aureus (S.aureus).It is anti- Bacterium peptide MDC can destroy bacterial cell membrane, or act on intracellular target site across cell membrane and kill bacterium in conjunction with lipopolysaccharides, right Gram-negative bacteria function and effect are better than gram positive bacteria.Tea polyphenols (Tea polyphenols, TP) also known as tea tannin, tea tannin, Victoria Polyphenols, antioxygen spirit, are the polyphenol mixtures extracted from tealeaves.Tea polyphenols in addition to stronger antioxidation, Also there is bactericidal effect to numerous food putrefactive microorganisms, and gram-negative bacteria is better than to gram positive bacteria function and effect, act on Mechanism is related to combining bacterial peptide glycan structures, destroys bacterium cell membrane, or act on bacterium specific target protein into the cell.In addition, tea is more Peculiar smell in the also adsorbable food of phenol, and there is protective effect to the pigment in food, inhibit the formation and accumulation of nitrite Effect.In early-stage study, we have found that antibacterial peptide MDC has synergistic effect with tea polyphenols for the first time, this is to improving tea polyphenols antibacterial Efficiency, expand tea polyphenols has great meaning as application range of the natural antibacterial antioxidant in food antiseptic.
Currently, not being used to prepare the correlation of antimicrobial preservative film about the antimicrobial component using antibacterial peptide MDC as preservative film Report.
Invention content
In order to solve the problems existing in the prior art, the purpose of the present invention is to provide a kind of edibility antimicrobial preservative film and its Preparation method.
It is another object of the present invention to provide the edibility antimicrobial preservative film food fresh keeping, food packaging and Application in tableware packaging.
To achieve the goals above, the present invention is achieved by the following technical programs：
A kind of edibility antimicrobial preservative film is prepared by the raw material of following weight percent meter：
Preferably, the edibility antimicrobial preservative film, which is characterized in that prepared by the raw material of following weight percent meter It forms：
Further, the amino acid sequence of the antibacterial peptide MDC such as SEQ ID NO:Shown in 1, specifically, the ammonia Base acid sequence is：GWLKKI GKKIE RVGQH TRDAT IQTIG VAQQA ANVAA TLKG.
Antibacterial peptide MDC provided by the invention is made using solid-state chemical reaction method method, specifically, is closed by Peptide synthesizer At polypeptide crude product；Then solid-phase synthesis synthesis polypeptide is used；The polypeptide of synthesis is carried out using reversed-phase high performance liquid chromatography again pure Change, and the polypeptide of synthesis is identified using electrospray mass spectrometry, to complete the preparation of polypeptide.
Further, the film forming agent is gelatine derivative.
Specifically, the gelatine derivative is prepared by the raw material of following weight percent meter：
Preferably, the gelatine derivative is prepared by the raw material of following weight percent meter：
Further, the sugar ester is in ocentyl succinic glucose ester, octadecenyl succinic acid-starch sugar ester It is at least one.
Further, the preparation of the gelatine derivative includes the following steps：
It weighs fishskin gelatin and is dissolved in purified water, be swollen 15~30min at room temperature, under the conditions of 35 DEG C, magnetic agitation 2~ 4h is made the solution that mass-volume concentration is 2~3%, is continuously heating to 60 DEG C, sugar ester is added under agitation, until molten Solution is complete, and epoxidized soybean oil is then slowly added dropwise, and mixes 5~10min, and Geniposide is added, and 1~2h of insulation reaction is cooled to room Temperature is dried under reduced pressure to get gelatine derivative.
Further, gelatine derivative prepares the fishskin gelatin of one of raw material and can be obtained by commercial sources, can also lead to It crosses conventional preparation method self-control to obtain, specifically, the preparation method of the fishskin gelatin includes the following steps：
(1) it scrapes peeling fish skin surface fish Scales and rejects the structure of fish muscle etc. adhered on fish-skin, and it is small that fish-skin is cut into 1 × 5cm Warm water is impregnated and is cleaned after item, removes grease and part soluble impurity, and by treated, fish-skin is dried, spare.
(2) fish-skin after 20g steps (1) are dried is weighed, 100ml saturation Ca (OH) are added2In solution, 7 are reacted in 4 DEG C of refrigerators Hour, liquid is periodically changed during reaction and interval whisks, and after the fish-skin after alkaline degradation is reacted is cleaned with deionized water, is added to In 100ml deionized waters, with NaOH and citric acid regulating solution pH=7, it is subsequently placed in heating water bath 8 in 60 DEG C of constant temperature water baths Hour, after carrying out thermal extraction, filtering dries filtrate to get fishskin gelatin.
Fishskin gelatin is directly as the filmogen of preservative film, and too strong, poor water resistance that there are water imbibitions, matter is crisp, mechanical property The problem of energy difference.The present invention substitutes fishskin gelatin with gelatine derivative, is used to prepare preservative film, the film mechanical performance of acquisition is notable Improve, and there is preferable water preventing ability.Specifically, by the way that a small amount of epoxidized soybean oil is added, the hydrophobic of epoxidized soybean oil is utilized Property so that the hydrophobicity of gelatin film is enhanced, and the moisture-vapor transmission of film can be effectively reduced.But the addition pair of epoxidized soybean oil The mechanical strength of gelatin film will produce detrimental effect, can reduce the tensile strength of gelatin film, reduce elongation at break, machinery Strength reduction.Unexpectedly, the inventors discovered that being compounded with epoxidized soybean oil and sugar ester, hydrophobic as fishskin gelatin changes Property agent use, under the crosslinked action of Geniposide, can overcome and be individually added into what epoxidized soybean oil brought gelatin film mechanical performance Adverse effect, makes the mechanical performance of acquisition preservative film significantly improve, and has higher water resistance.It should be noted that only and work as institute The sugar ester stated is the anionic surfactant that HLB value is 12~16, specially ocentyl succinic glucose ester or 18 The mixture of starch alkenyl succinate sugar ester or both could obtain above-mentioned effect.Remaining nonionic surfactants sugar Ester such as sucrose fatty ester, maltol aliphatic ester or milk sugar fats acid esters, cannot obtain above-mentioned effect.
In addition, the present invention also provides a kind of methods of the edibility antimicrobial preservative film comprising following steps：
(1) film forming agent is weighed, purified water is dissolved in, the film forming solution that mass-volume concentration is 4% is made, is then added sweet Oil stirs 30min, sequentially adds antibacterial peptide MDC, tea polyphenols and Tween-80, stir evenly, obtain composite membrane liquid；
(2) composite membrane liquid is placed under conditions of vacuum degree is 0.08~0.09MPa and is de-gassed 3~6min, repeated de- After gas 3 times, stands 0.5~1h and remove bubble removing, obtain filming emulsion；
(3) filming emulsion is inclined and is placed on organic glass tablet, it is dry under the conditions of spontaneously drying or being placed in 30~60 DEG C, i.e., Obtain edibility antimicrobial preservative film.
Preservative film provided by the invention selects the tea polyphenols with synergetic antibacterial effect and antibacterial peptide MDC is antiseptic, can Effectively to inhibit the growth of common microbiological in food, Escherichia coli, staphylococcus aureus, salmonella are all had preferably Bacteriostasis, extend food antiseptic freshness date.The antibacterial peptide MDC is a kind of insect antimicrobial peptide of this seminar clone, Mechanism of action is unique, is not likely to produce drug resistance.Tea polyphenols are the polyphenol mixtures extracted from tealeaves, have it is anti-oxidant and Antibacterial action.There is complementary collaboration in the two antibacterial mechanisms, learn from other's strong points to offset one's weaknesses, and the drug resistance for solving microorganism especially bacterium is asked Topic has good reference function, while these provide new think of from natural biological bacteriostatic agent to solve food-safety problem Road.
Compared with prior art, the invention has the advantages that：
(1) edibility antimicrobial preservative film or its decomposition product provided by the invention are nontoxic, safe, have preferable Anti-microbial property, it is notable to common food microorganisms antibacterial action, and mechanical performance is good, have stronger tensile strength and compared with Big elongation at break, the application suitable for food fresh keeping, food packaging and tableware packaging.
(2) present invention is used in compounding using antibacterial peptide MDC and tea polyphenols as antiseptic, and the two has cooperative gain effect, It can be obtained preferable anti-bacterial refreshing effect under lower usage amount, the antibacterial effect of the two is better than antibacterial peptide MDC- Chinese cassia trees The effect that aldehyde, antibacterial peptide MDC- eugenols and aggressin (Attacins)-tea polyphenols are applied in combination, and greatly reduce and be produced into This.
Description of the drawings
Fig. 1 is the high-efficient liquid phase chromatogram of antibacterial peptide MDC.
Fig. 2 is the mass spectrogram of antibacterial peptide MDC.
Fig. 3 is that the smooth densification of scanning electron microscopic observation edibility anti-bacterial refreshing film surface is evenly distributed.
Specific implementation mode
The present invention is made with specific embodiment with reference to the accompanying drawings of the specification and further being elaborated, the embodiment It is served only for explaining the present invention, be not intended to limit the scope of the present invention.Test method used in following embodiments is such as without spy Different explanation, is conventional method；Used material, reagent etc., unless otherwise specified, for the reagent commercially obtained And material.
1 solid-state chemical reaction method method synthetic antibacterial peptide MDC of embodiment
The amino acid sequence of antibacterial peptide MDC is：Ac-GWLKKI GKKIE RVGQH TRDAT IQTIG VAQQA ANVAA TLKG-NH2, such as SEQ ID NO:Shown in 1, contain 40 amino acid, theoretical isoelectric point is 10.56, and theoretical molecular weight is 4299.04.The preparation of antibacterial peptide MDC carries out one by one from C-terminal to N-terminal, is completed by Peptide synthesizer, the specific steps are：
(1) Fmoc-X (X is first amino acid of antibacterial peptide MDC C-terminals) is linked into Wang resins first, then taken off X-Wang resins are obtained after removing Fmoc groups；By Fmoc-Y-Trt-OH, (9- fluorenes methoxy carboxyl-trimethyl-Y, Y is antibacterial peptide again Second amino acid of MDC C-terminals)；It is synthesized to N-terminal from C-terminal successively according to this program, until synthesis finishes, obtains sloughing Fmoc The resin of the side chain protection of group；
(2) in peptide resin obtained above, cutting reagent is added, 20 DEG C are protected from light lower reaction 2h, filtering；Precipitation TFA (trifluoroacetic acid) washs, and washing lotion is mixed with above-mentioned filtrate, and Rotary Evaporators concentration adds the precooling nothing of 10 times or so volumes Water ether, -20 DEG C of precipitation 3h, is precipitated white powder object, centrifuges 10min with 2500g, collects precipitation, then washed with anhydrous ether Precipitation, vacuum drying, obtains polypeptide, wherein cutting reagent by TFA, water and TIS (tri isopropyl chlorosilane) according to mass ratio 95: 2.5:2.5 mixing；
(3) 0.2mol/L sodium sulphate (phosphoric acid is adjusted to pH7.5) is used to carry out column equilibration 30min, with 90% aqueous acetonitrile Liquid dissolves polypeptide, and filtering, C18 reverse phase normal pressure columns, using gradient elution, (eluant, eluent is methanol and aqueous sodium persulfate solution according to volume Than being 30:70~70:30 mixing), flow velocity 1mL/min, detection wave is 220nm, collects main peak, freeze-drying；
(4) reverse phase C18 columns are recycled to be further purified, eluent A is 0.1%TFA/ aqueous solutions；Eluent B is 0.1% TFA/ acetonitrile solutions, wash-out concentration is 25%B~40%B, elution time 12min, flow velocity 1mL/min, then is ibid collected Main peak is lyophilized to get refined antibacterial peptide MDC；
(5) refined antibacterial peptide MDC is obtained by reversed-phase high performance liquid chromatography and electron spray mass spectrometry analysis, reverse phase by above-mentioned High-efficient liquid phase chromatogram as shown in Figure 1, mass spectrogram as shown in Fig. 2, the results show that the purity of antibacterial peptide MDC be more than 95%, molecule Amount is 4299.36, almost the same with theoretical molecular weight.
It is prepared by 2 gelatine derivative of embodiment
Gelatine derivative prepare raw material and its composition is as shown in the table：
The preparation of A group gelatine derivatives：
It weighs fishskin gelatin and is dissolved in purified water, be swollen 25min at room temperature, under the conditions of 35 DEG C, magnetic agitation 2.5h is made The solution that mass-volume concentration is 2%, is continuously heating to 60 DEG C, sugar ester is added under agitation, until dissolving is complete, then Be slowly added dropwise epoxidized soybean oil, mix 6min, Geniposide is added, insulation reaction 1.5h is cooled to room temperature, be dried under reduced pressure to get Gelatine derivative.
The preparation of B-F group gelatine derivatives refers to A groups.
Embodiment 3-7 edibility anti-bacterial refreshing film preparations
Edibility antimicrobial preservative film prepare raw material and its composition is as shown in the table：
Preparation method：
(1) film forming agent is weighed, purified water is dissolved in, the film forming solution that mass-volume concentration is 4% is made, is then added sweet Oil stirs 30min, sequentially adds antibacterial peptide MDC, tea polyphenols and Tween-80, stir evenly, obtain composite membrane liquid；
(2) composite membrane liquid is placed under conditions of vacuum degree is 0.09MPa and is de-gassed 5min, repeated after deaerating 3 times, it is quiet It sets to 0 .5~1h and removes bubble removing, obtain filming emulsion；
(3) filming emulsion is inclined and is placed on organic glass tablet, dried to get can under the conditions of spontaneously drying or being placed in 45 DEG C Feeding habits antimicrobial preservative film.
Comparative example 1-6 edibility anti-bacterial refreshing film preparations
Edibility antimicrobial preservative film prepare raw material and its composition is as shown in the table：
Preparation method refers to above-described embodiment.
Test example one, scanning electron microscope observation (SEM)
Using the surface condition of edibility antimicrobial preservative film made from scanning electron microscopic observation embodiment 3, specially：Using leading The antibacterial membrane sample for being cut into 6mm × 6mm sizes is fixed on sample stage by electric adhesive tape, after metal spraying is handled, uses scanning electricity The surface appearance feature of sub- microscope (SEM) observation film.Scanning electron microscope is observation thin-film material surface microscopic appearance Most common means, using scanning electron microscope (HITACHI S-3400N types), emitting voltage 20KV passes through magnetic lenses It focuses electron beam and forms electron probe, scan to obtain electronic signal in specimen surface, be finally converted into material through kinescope again Pattern displays, and the results are shown in Figure 3：The smooth densification of edibility anti-bacterial refreshing film surface made from embodiment 3, distribution are equal It is even.
Test example two, film thickness determination
The thickness for measuring edibility antimicrobial preservative film made from embodiment 3-7 and comparative example 1-6 respectively using thickness gauge, 5 points of random test, measuring accuracy 1um are averaged on film sample.The results show that 3-7 of the embodiment of the present invention and comparative example 1- The film thickness of edibility antimicrobial preservative film is within the scope of 51.5~59.7um made from 6
Test example three, Measuring Mechanical Properties
Edibility antibacterial made from embodiment 3-7 and comparative example 1-3 is measured respectively according to national standard GBT 1040.3-2006 to protect The mechanical performance of fresh film, antimicrobial preservative film are cut into 120 × 20mm sizes, use electronic universal tester test film mechanicalness Can, load 500N is arranged between fixture and initially presss from both sides away from for 40mm, tensile speed 5mm/min, measures tensile strength and extension at break Rate takes the average value of 5 repetition experimental results, and the results are shown in Table 1.
The Measuring Mechanical Properties result of 1 antimicrobial preservative film of table
Group Tensile strength (MPa) Elongation at break (%)
Embodiment 3 55.37±3.67**##▲▲ 51.3
Embodiment 4 53.16±3.45**##▲▲ 49.8
Embodiment 5 56.84±4.30**##▲▲ 52.4
Embodiment 6 53.72±4.53**##▲▲ 50.0
Embodiment 7 54.15±3.98**##▲▲ 50.9
Comparative example 1 40.52±2.12 36.4
Comparative example 2 39.75±2.44 34.8
Comparative example 3 30.26±3.15 24.5
Note：Compared with comparative example 1,**P ＜ 0.01；Compared with comparative example 2,##P ＜ 0.01；Compared with comparative example 3,▲▲P ＜ 0.01。
The results show that the tensile strength and elongation at break of edibility antimicrobial preservative film made from 3-7 of the embodiment of the present invention It is superior to comparative example 1-3, there is preferable mechanical performance.The above result shows that with ocentyl succinic glucose ester or 18 Starch alkenyl succinate sugar ester or both mixture is used in compounding gelatine derivative obtained with epoxidized soybean oil, is used to prepare anti- Bacterium preservative film has preferable mechanical performance.
Test example four, water vapo(u)r transmission measure
The water vapo(u)r transmission of edibility antimicrobial preservative film made from embodiment 3-7 and comparative example 1-3 is measured respectively, specifically For：The edibility antimicrobial preservative film precision chosen is covered on the measuring cup equipped with distilled water, seals, is put into close drying In device (relative humidity 0%), keep film inside and outside vapour pressure deficit, and by drier be put into constant temperature and humidity think (25 DEG C, In 50%RH), weighed once every 1h, nominal amount 10 times, quality measurement loss amount changes with time, and drafting pattern, obtains To R2 >=0.99, parallel determination three times, is calculated as follows：
Vapor transmission coefficient WVP/ (g.mm/ (KPa.h.m2))=(K × L)/(A × △ P), in formula, K is slope, and L is Thickness/mm of film, A are the area m for measuring film2, △ P take 3.168kPa.
The results are shown in Table 2.
The moisture-vapor transmission measurement result of 2 antimicrobial preservative film of table
Group Moisture-vapor transmission (g.mm/m2.h.kPa)
Embodiment 3 0.187±0.03*#
Embodiment 4 0.204±0.02*#
Embodiment 5 0.179±0.04*#
Embodiment 6 0.196±0.03*#
Embodiment 7 0.190±0.02*#
Comparative example 1 0.249±0.04
Comparative example 2 0.240±0.03
Comparative example 3 0.175±0.05
Note：Compared with comparative example 1,*P ＜ 0.05；Compared with comparative example 2,#P ＜ 0.05.
The results show that edibility antimicrobial preservative film made from 3-7 of the embodiment of the present invention there is lower vapor to penetrate Rate is better than comparative example 1-2.By comparative example 1 and 2 it is found that replacing the pungent of the present invention with sucrose fatty ester or milk sugar fats acid esters Alkenyl succinic acid glucose ester or octadecenyl succinic acid-starch sugar ester or both mixture, are used to prepare gelatine derivative, most The moisture-vapor transmission of the antimicrobial preservative film obtained eventually is increased slightly, and shows that the sugar ester of nonionic can influence epoxidized soybean oil Hydrophobicity, comparative example 3 it is found that the vapor of the antimicrobial preservative film finally being obtained without gelatine derivative made of sugar ester is saturating It is little to cross rate variation, shows that the sugar ester of anionic does not influence the hydrophobicity of epoxidized soybean oil.
Test example five, anti-microbial property measure
The anti-microbial property of edibility antimicrobial preservative film made from embodiment 3,6,7 and comparative example 4-6 is measured respectively, specifically For：Inhibition of the preservative film to Escherichia coli, staphylococcus aureus, salmonella is measured by filter paper inhibition zone method. 0.1mL bacterium number amounts a concentration of 10 are drawn with liquid-transfering gun6It is the Escherichia coli of CFU/mL, staphylococcus aureus, salmonella, waxy Bacillus suspension is inoculated in nutrient agar, even spread.Then the different film liquids of 7 μ L are drawn respectively in ultraviolet-sterilization On filter paper (a diameter of 6mm) afterwards, culture plate is placed in 37 DEG C of incubator cultures for 24 hours, and the filter paper to add sterile water is sky White control, measures antibacterial region, replication 3 times.
Antibacterial region/mm2=inhibition zone area/mm2Filter paper area/mm2。
The results are shown in Table 3.
The anti-microbial property measurement result of 3 antimicrobial preservative film of table
Note：Compared with comparative example 4,**P ＜ 0.01；Compared with comparative example 5,#P ＜ 0.05；Compared with comparative example 6,▲P ＜ 0.05。
The results show that edibility antimicrobial preservative film made from the embodiment of the present invention 3,6,7 to Escherichia coli, golden yellow Portugal Grape coccus and salmonella all have preferable fungistatic effect, are better than comparative example 4-6.By comparative example 4 it is found that being attacked with antibacterial peptide Plain (Attacins) replaces the antibacterial peptide MDC of the present invention and tea polyphenols compounding is used as antiseptic, to Escherichia coli, Salmonella Bacterium still has preferable antibiotic property, but poor to the anti-microbial property of staphylococcus aureus, substantially less than embodiment 3,6,7.By Comparative example 5,6 uses it is found that replacing tea polyphenols using cinnamic acid and eugenol respectively and being compounded as antiseptic with antibacterial peptide MDC, right The anti-microbial property of Escherichia coli, staphylococcus aureus and salmonella declines, and is less than embodiment 3,6,7.The above result shows that Antibacterial peptide MDC and tea polyphenols provided by the invention have synergetic antibacterial effect, effect more better than aggressin (Attacins)-tea The using effect of phenol, antibacterial peptide MDC- cinnamic acids, antibacterial peptide MDC- eugenols.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair The limitation of the present invention, protection scope of the present invention should be subject to claim limited range.For the art For those of ordinary skill, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, these change Protection scope of the present invention is also should be regarded as into retouching.
Sequence table
<110>Guangdong pharmaceutical university
<120>A kind of edibility antimicrobial preservative film and its preparation method and application
<130> 111
<160> 1
<170> SIPOSequenceListing 1.0
<210> 1
<211> 40
<212> PRT
<213>Artificial sequence (Artificial Sequence)
<400> 1
Gly Thr Leu Leu Leu Ile Gly Leu Leu Ile Gly Ala Val Gly Gly His
1 5 10 15
Thr Ala Ala Ala Thr Ile Gly Thr Ile Gly Val Ala Gly Gly Ala Ala
20 25 30
Ala Val Ala Ala Thr Leu Leu Gly
35 40

Claims (10)

1. a kind of edibility antimicrobial preservative film, which is characterized in that be prepared by the raw material of following weight percent meter：
2. edibility antimicrobial preservative film according to claim 1, which is characterized in that by the raw material of following weight percent meter It is prepared：
3. edibility antimicrobial preservative film according to claim 1 or 2, which is characterized in that the amino of the antibacterial peptide MDC Acid sequence such as SEQ ID NO:Shown in 1.
4. edibility antimicrobial preservative film according to claim 1 or 2, which is characterized in that the film forming agent spreads out for gelatin Biology.
5. edibility antimicrobial preservative film according to claim 4, which is characterized in that the gelatine derivative is by following heavy The raw material of amount percentages is prepared：
6. edibility antimicrobial preservative film according to claim 5, which is characterized in that the gelatine derivative is by following heavy The raw material of amount percentages is prepared：
7. edibility antimicrobial preservative film according to claim 5 or 6, which is characterized in that the sugar ester is octenyl amber At least one of amber sour grapes sugar ester, octadecenyl succinic acid-starch sugar ester.
8. edibility antimicrobial preservative film according to claim 5 or 6, which is characterized in that the system of the gelatine derivative It is standby to include the following steps：
It weighs fishskin gelatin and is dissolved in purified water, be swollen 15~30min at room temperature, under the conditions of 35 DEG C, 2~4h of magnetic agitation, system The solution for being 2~3% at mass-volume concentration, is continuously heating to 60 DEG C, sugar ester is added under agitation, until having dissolved Entirely, epoxidized soybean oil is then slowly added dropwise, mixes 5~10min, Geniposide is added, 1~2h of insulation reaction is cooled to room temperature, subtracts It press dry dry to get gelatine derivative.
9. a kind of method preparing the edibility antimicrobial preservative film as described in claim 1-8 is any, which is characterized in that including with Lower step：
(1) film forming agent is weighed, purified water is dissolved in, the film forming solution that mass-volume concentration is 4% is made, glycerine is then added, 30min is stirred, antibacterial peptide MDC, tea polyphenols and Tween-80 is sequentially added, stirs evenly, obtain composite membrane liquid；
(2) composite membrane liquid is placed under conditions of vacuum degree is 0.08~0.09MPa and is de-gassed 3~6min, repeat degassing 3 times Afterwards, it stands 0.5~1h and removes bubble removing, obtain filming emulsion；
(3) filming emulsion is inclined and is placed on organic glass tablet, dried to get can under the conditions of spontaneously drying or being placed in 30~60 DEG C Feeding habits antimicrobial preservative film.
10. being packed in food fresh keeping, food packaging and tableware according to any edibility antimicrobial preservative films of claim 1-9 In application.
CN201810054727.6A 2018-01-19 2018-01-19 Edible antibacterial preservative film and preparation method and application thereof Active CN108395705B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810054727.6A CN108395705B (en) 2018-01-19 2018-01-19 Edible antibacterial preservative film and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810054727.6A CN108395705B (en) 2018-01-19 2018-01-19 Edible antibacterial preservative film and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN108395705A true CN108395705A (en) 2018-08-14
CN108395705B CN108395705B (en) 2020-05-08

Family

ID=63094994

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810054727.6A Active CN108395705B (en) 2018-01-19 2018-01-19 Edible antibacterial preservative film and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN108395705B (en)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109679355A (en) * 2018-12-14 2019-04-26 华南农业大学 A kind of antibacterial film and its application
CN110432422A (en) * 2019-07-10 2019-11-12 中国农业科学院农产品加工研究所 A kind of edibility bacteriostatic film agent and preparation method thereof and application
CN110684361A (en) * 2019-08-19 2020-01-14 浙江海洋大学 Preparation method of glucose-modified gelatin edible preservative film
CN111073308A (en) * 2019-12-26 2020-04-28 汕头大学 Gelatin-based food packaging film and preparation method thereof
CN111423604A (en) * 2020-03-20 2020-07-17 江西师范大学 Preparation method of ultrasonic modified composite gelatin film
CN112920471A (en) * 2021-02-26 2021-06-08 杭州拜迪戈雷生物材料有限公司 Antibacterial water-resistant material and preparation method thereof
CN114854217A (en) * 2022-06-16 2022-08-05 陕西科技大学 Biodegradable water-repellent anti-ultraviolet gelatin-based bioplastic film and preparation method thereof
CN115304801A (en) * 2021-05-07 2022-11-08 西安理工大学 Application of edible insect protein in packaging film
CN115606596A (en) * 2022-11-02 2023-01-17 中国石油大学(华东) Reticular antibacterial material, preparation method and application thereof
CN115777764A (en) * 2022-10-21 2023-03-14 自然资源部第三海洋研究所 Edible coating liquid, composite edible film, composite coating liquid, and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010124821A (en) * 2008-11-25 2010-06-10 Bio Verde:Kk Antibacterial preserving liquid
CN106750576A (en) * 2016-12-05 2017-05-31 深圳职业技术学院 A kind of Antibacterial composite preservative film and preparation method thereof
CN107183144A (en) * 2017-05-17 2017-09-22 西北农林科技大学 A kind of application of composite preservative and its fresh-keeping Chilled Meats

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010124821A (en) * 2008-11-25 2010-06-10 Bio Verde:Kk Antibacterial preserving liquid
CN106750576A (en) * 2016-12-05 2017-05-31 深圳职业技术学院 A kind of Antibacterial composite preservative film and preparation method thereof
CN107183144A (en) * 2017-05-17 2017-09-22 西北农林科技大学 A kind of application of composite preservative and its fresh-keeping Chilled Meats

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109679355A (en) * 2018-12-14 2019-04-26 华南农业大学 A kind of antibacterial film and its application
CN110432422A (en) * 2019-07-10 2019-11-12 中国农业科学院农产品加工研究所 A kind of edibility bacteriostatic film agent and preparation method thereof and application
CN110684361B (en) * 2019-08-19 2021-08-20 浙江海洋大学 Preparation method of glucose-modified gelatin edible preservative film
CN110684361A (en) * 2019-08-19 2020-01-14 浙江海洋大学 Preparation method of glucose-modified gelatin edible preservative film
CN111073308A (en) * 2019-12-26 2020-04-28 汕头大学 Gelatin-based food packaging film and preparation method thereof
CN111423604A (en) * 2020-03-20 2020-07-17 江西师范大学 Preparation method of ultrasonic modified composite gelatin film
CN111423604B (en) * 2020-03-20 2022-05-20 江西师范大学 Preparation method of ultrasonic modified composite gelatin film
CN112920471A (en) * 2021-02-26 2021-06-08 杭州拜迪戈雷生物材料有限公司 Antibacterial water-resistant material and preparation method thereof
CN115304801A (en) * 2021-05-07 2022-11-08 西安理工大学 Application of edible insect protein in packaging film
CN114854217A (en) * 2022-06-16 2022-08-05 陕西科技大学 Biodegradable water-repellent anti-ultraviolet gelatin-based bioplastic film and preparation method thereof
CN115777764A (en) * 2022-10-21 2023-03-14 自然资源部第三海洋研究所 Edible coating liquid, composite edible film, composite coating liquid, and preparation method and application thereof
CN115606596A (en) * 2022-11-02 2023-01-17 中国石油大学(华东) Reticular antibacterial material, preparation method and application thereof
CN115606596B (en) * 2022-11-02 2024-02-23 中国石油大学(华东) Reticular antibacterial material, preparation method and application thereof

Also Published As

Publication number Publication date
CN108395705B (en) 2020-05-08

Similar Documents

Publication Publication Date Title
CN108395705A (en) A kind of edibility antimicrobial preservative film and its preparation method and application
Cui et al. Biodegradable zein active film containing chitosan nanoparticle encapsulated with pomegranate peel extract for food packaging
Hajji et al. Conception of active food packaging films based on crab chitosan and gelatin enriched with crustacean protein hydrolysates with improved functional and biological properties
Kalkan et al. Physicochemical and bioactive properties of edible methylcellulose films containing Rheum ribes L. extract
Li et al. Development of antibacterial ε-polylysine/chitosan hybrid films and the effect on citrus
Kchaou et al. Bioactive films based on cuttlefish (Sepia officinalis) skin gelatin incorporated with cuttlefish protein hydrolysates: Physicochemical characterization and antioxidant properties
Wang et al. Composite chitosan films prepared using nisin and Perilla frutescense essential oil and their use to extend strawberry shelf life
Yun et al. Development of chitosan films incorporated with rambutan (Nephelium lappaceum L.) peel extract and their application in pork preservation
CN104126656A (en) Chitosan-orange peel essential oil composite plastic wrap with bacteriostasis functions
CN114014923B (en) Scylla paramamosain antibacterial polypeptide Sp-LECin and application thereof
CN109679355A (en) A kind of antibacterial film and its application
Zhang et al. Antibacterial activity of water-phase extracts from bamboo shavings against food spoilage microorganisms
Alnadari et al. A new natural drying method for food packaging and preservation using biopolymer-based dehydration film
Radhalakshmi et al. Development of active packaging film based on poly (lactic acid) incorporated with Piper betel leaf ethanolic extract and its application in the shelf-life extension of tuna meat
Guo et al. Fabrication and characterization of sodium alginate/blueberry anthocyanins/hinokitiol loaded ZIF-8 nanoparticles composite films with antibacterial activity for monitoring pork freshness
Wang et al. Preparation of eco-friendly composite food packaging films based on gelatin and a matrine coconut acids ionic liquid
Rad et al. Preparation and characterization of pullulan-soy protein concentrate blended film incorporated with Zataria multiflora and Artemisia biennis essential oils
CN106674331B (en) Antibacterial lipopeptide bacaucin and preparation method and application thereof
Khalil et al. Evaluation of the physicochemical properties and antimicrobial activities of bioactive biodegradable films
CN103120200A (en) Preparation method of water-soluble olive polyphenol with bacteriostatic and preserved activity on meat products
CN109430687A (en) A kind of composition can be used as aflatoxin scavenger
CN108931408A (en) A kind of anatomic teaching sample guarantor&#39;s color fixing liquid and preparation method thereof
Pandurangan et al. Evaluation of antimicrobial and anthelmentic activity of leaves of Chromolaena odorata
CN115340712A (en) Functional edible composite film based on pullulan and preparation method thereof
KR102204369B1 (en) Method for manufacturing collagen with improved odor and viscosity and food composition and cosmetic composition using the same

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20210730

Address after: 200000 room p366, building 7, No. 228, jingle Road, Langxia Town, Jinshan District, Shanghai

Patentee after: Shanghai YunRuo Biotechnology Co.,Ltd.

Address before: 510006 40 Haizhuqu District, Guangdong, Guangzhou.

Patentee before: GUANGDONG PHARMACEUTICAL University

TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20230802

Address after: 201600 Building 1, 1128 Wenhui Road, Songjiang District, Shanghai

Patentee after: Shanghai Digital Entropy Dimension Medical Information Technology Co.,Ltd.

Address before: 200000 room p366, building 7, No. 228, jingle Road, Langxia Town, Jinshan District, Shanghai

Patentee before: Shanghai YunRuo Biotechnology Co.,Ltd.