CN103554532A - Ferulic acid-collagen antibacterial film and preparation method and application thereof - Google Patents
Ferulic acid-collagen antibacterial film and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a ferulic acid-collagen antibacterial film and a preparation method and application thereof. The preparation method comprises the steps of adding collagen into water, stirring and dissolving at the heat treatment temperature of 60-70 ℃, sequentially adding glycerol, dialdehyde starch, sodium alginate and ferulic acid, carrying out heat treatment at the temperature of 60-70 ℃ for 20-30 minutes, placing in a stirring defoaming machine to remove bubbles, carrying out tape casting on an organic glass plate, drying after the film forming solution is cooled, cooling at normal temperature, and uncovering to obtain the ferulic acid-collagen antibacterial film. The edible food packaging film prepared by the invention has the advantages of high transparency, good barrier property, high mechanical strength and antibacterial property, and the diameter of a gram-negative bacteria inhibition zone and a gram-positive bacteria inhibition zone of the film obtained by the Oxford cup method is 17-22mm, so that the film has strong antibacterial ability. The prepared film is used for preserving the sausage, and can prolong the shelf life of the sausage by 8.5 days.
Description
Technical field
The present invention relates to a kind of fresh-keeping antibacterial film, particularly relate to a kind of forulic acid-collagen protein antibacterial film and preparation method thereof and application on food preservation, belong to the green manufacture field of food.
Background technology
Edibility antibacterial film not only has the food spoilage of preventing, reduces the growth of spoilage microorganisms, improves Food storage stability, extends the function of Food Shelf-life; Can also reduce and even avoid directly adding of sanitas in food processing process, ensure human consumer's edible safety; Simultaneously also biodegradable, can not cause the environmental problem of packaging waste pollution, and become the developing direction of food antiseptic packaging industry.
Meat product occupies epochmaking status in the daily meals of people, for keeping the storage stability of meat product, conventionally need in food preservation, add a large amount of sanitass, but the interpolation of sanitas has brought safely larger hidden danger also to meat product.The development of edibility antibacterial film, not only can improve meat product storage stability, can also reduce and even avoid directly adding of sanitas in the meat product course of processing.Can be used as the carrier of meat product flavour agent, antioxidant and anti-microbial agents etc. simultaneously, be applied to plastics packed internal layer, reduce and prevent that the Harmful Residue in plastics is to the migration in meat product, ensure human consumer's edible safety, and class coating material is protein substance, except edible, also have certain nourishing function, meat product industry aspect has broad application prospects.
Zhang Meiyun, Liu Liu etc., the Application and research progress of collagen film [J], Chinese leather, 2007,36 (3): 39-41, utilize collagen protein to be combined and to make blend film with carboxymethyl cellulose, its mechanical property still can, but anti-microbial property is poor.
Chinese invention patent application 201210118934.6 discloses a kind of antioxidant collagen protein-active film and preparation method who contains plant milk extract, belongs to edible film blending and modifying field.In the anti-oxidant activity membrane component of this invention, contain plant milk extract, collagen protein, glycerine; During preparation, first collagen protein and glycerine are dissolved in to distilled water in proportion and make collagen aqueous solution, then add distilled water to make solution plant milk extract, then add a certain amount of in collagen liquid, stir, ultrasonic degas, pipettes and spreads in drying and forming-film on poly (methyl methacrylate) plate.Activated protein film prepared by the present invention is compared with simple collagen film; due to adding of extract; oxidation-resistance obviously improves; and there is good ultraviolet isolating performance and certain germ resistance; in addition it is wet that this protein film also has resistance; gas barrier properties, degradable, thus reach protection food and the effect that reduces environmental pollution.But the mechanical property of this collagen film has much room for improvement, germ resistance is not strong yet.
The chemical name of forulic acid (Ferulic Acid) is 4 hydroxyl 3 methoxy cinnamic acids, is one of derivative of TRANSCINNAMIC ACID (claiming again styracin, 3 phenyl 2 vinylformic acid, molecular structure).Forulic acid has platelet aggregation-against, suppresses platelet 5-HT and discharges, and suppresses platelet thrombus element a2(txa2) generation, strengthen prostaglandin(PG) active, analgesia, the effects such as alleviating vascular spasm.To produce the basic raw material that is used for the treatment of the disease medicines such as cardiovascular and cerebrovascular diseases and oligoleukocythemia.Forulic acid also has the effect of stronger anti-oxidation protection DNA.But not yet there is the report that forulic acid and collagen protein is prepared to antibacterial film.
Summary of the invention
The object of the invention is to the problem for prior art packaging material for food, provide a kind of anti-bacterial refreshing ability strong, good mechanical property, there is forulic acid-collagen protein antibacterial film of edibility and preparation method thereof.
Another object of the present invention is to provide the application of above-mentioned forulic acid-collagen protein antibacterial film on food preservation.
It is base-material that collagen protein and forulic acid are take in the present invention, is equipped with glycerine, dialdehyde starch and sodium alginate, in the strict bubbles volume condition of controlling temperature and solution, and preparation forulic acid-collagen protein antibacterial film.
Object of the present invention is achieved through the following technical solutions:
A kind of preparation method of forulic acid-collagen protein antibacterial film: collagen protein is added to the water, in thermal treatment temp, it is stirring and dissolving under 60 ℃～70 ℃ conditions, add successively glycerine, dialdehyde starch, sodium alginate and forulic acid, thermal treatment 20-30 minute under 60 ℃～70 ℃ conditions, be placed in and stir defoamer and slough bubble, then on poly (methyl methacrylate) plate curtain coating, liquid cooling to be filmed is post-drying but, cooling under normal temperature, take off film, make forulic acid-collagen protein antibacterial film; In the mass concentration in solution, collagen concentration is 6-14%, and forulic acid is 0.06-0.70%, and glycerine is 1.20-5.60%, and dialdehyde starch is 0.12-1.40%, sodium alginate 0.24-1.68%.
For further realizing the object of the invention, preferably, described oven dry is to be placed in the baking oven of 60 ℃ to toast 4-6h.In the mass concentration in solution, described collagen concentration is 8-12%.Described glycerol concentration is 1.60-3.60%.Described sodium alginate concentration is 0.40-0.84%.Described dialdehyde starch concentration is 0.32-0.60%.Described forulic acid concentration is 0.16-0.36%.
-collagen protein antibacterial film, is prepared by aforesaid method.
The application of forulic acid-collagen protein antibacterial film on food preservation.
The present invention finds that forulic acid and collagen protein have good film-forming properties while being mixed, add a certain amount of glycerine, dialdehyde starch and sodium alginate, forulic acid-collagen protein antibacterial film the mechanical property obtaining is excellent especially, and when thickness is 0.21 millimeter, tensile strength reaches 1.80-2.03MPa; Elongation at break is 98.12%-118.73%; Forulic acid can be reacted and make protein cross with Methionin in protein, halfcystine, tyrosine etc., adds water vapor, oxygen and carbonic acid gas transmitance that microdose of ferulic acid can improve the mechanical property of film and reduce film in film-forming soln.In addition, forulic acid is as a kind of broad spectrum, natural antibacterial agent, also give film with anti-microbial property, it is 17-22mm to the antibacterial circle diameter of Gram-negative bacteria (intestinal bacteria) and Gram-positive (staphylococcus) that Oxford agar diffusion method records gained film, show very strong bacteriostasis, by this film be coated on sausage fresh-keeping in, can be by sausage shelf life extension 8.5 days.In addition, dialdehyde starch can play crosslinking reaction with amino in collagen protein and imino-, has improved mechanical property and the barrier property of film, has avoided general edible film to use the interpolation of the compositions such as glutaraldehyde and epoxy chloropropane, really accomplishes edible.
In the mass concentration in solution, in the present invention in the full span of glycerol concentration and dialdehyde starch concentration, the variation tendency of elongation at break is: when glycerol concentration is lower than 0 level (30%), along with the increase of glycerine addition, raise, when glycerine addition is during higher than 0 level, along with the increase of glycerine addition, decline; Equally, when the addition of valeral is on close level with 0 gradually, elongation at break also increases thereupon.The interaction of glycerol concentration and dialdehyde starch concentration reflects that suitable condition can make elongation at break reach maximum value, but the too high or too low elongation at break that all can make reduces.
In the mass concentration in solution, the significant interaction of glycerol concentration and forulic acid concentration in the present invention, the variation of glycerol concentration on the impact of elongation at break slightly higher than forulic acid.During beginning, with the rising of glycerol concentration and forulic acid concentration, elongation at break increases thereupon, but when glycerol concentration and forulic acid concentration are increased to a certain degree, it is maximum that elongation at break also reaches; When glycerol concentration and forulic acid concentration continuation rising, elongation at break starts to decline.Be glycerol concentration and forulic acid excessive concentration or when too low, elongation at break all can not reach maximum value.
In the mass concentration in solution, in the present invention, along with the increase of dialdehyde starch concentration and forulic acid concentration, elongation at break is in continuous increase, and after dialdehyde starch concentration and forulic acid concentration increase to a certain degree, it is maximum that elongation at break reaches; When dialdehyde starch concentration and forulic acid concentration continue to raise, elongation at break can decline again thereupon.By surface chart, can be found out, when glycerol concentration keeps certain (0.15%), pentanediol concentration is greater than forulic acid to the impact of elongation at break.
Glycerine, as a kind of softening agent, not only can improve the processing characteristics of protein film, and larger on the mechanical property impact of film.Do not add or only add the glycerine of minute quantity, the easy embrittlement of film becoming.A certain amount of glycerine can make the mechanical property of collagen film be improved, and excessive interpolation can make film become extremely soft on the contrary, deformability obviously increases, tensile strength obviously reduces, this is because glycerine strengthens to the weakening of Hyarogen-bonding in gelling system and to the diluting effect of protein molecular, causes the tensile strength of collagen film to produce variation.Glycerol concentration is between 1.25% and 1.65%, collagen film tensile strength and elongation at break all peak, glycerol concentration is too low, collagen film is easily crisp easily broken, when glycerol concentration is too high, no matter collagen film is that elongation at break or tensile strength have the downtrending of presenting, and collagen film is difficult for dry, surface viscosity is large, and water-absorbent is strong.
When sodium alginate concentration is lower, institute's film forming denseness is low, and viscosity is poor, and bad mechanical property easily shrinks fracture while taking off film, be difficult to take off film.Because the relative molecular mass of sodium alginate is larger, molecular chain is also longer, and macromolecular chain forms a random ball of string, easily tangle to each other, the result of entanglement makes flow unit become large, has increased the resistance of flow, thereby can cause viscosity to increase, affected the film degree of taking off.Sodium alginate concentration is larger, and the viscosity of solution is also larger, and its ventilation property is just less, when concentration reach 0.50% or more than, prepared collagen film starts there is bubble, its mechanical property also declines thereupon; 0.30%～0.40% is its comparatively suitable concentration range.
Dialdehyde starch concentration has larger impact to the physical strength of film, and along with the increase of dialdehyde starch content, physical strength first increases last decline of then tending towards stability, and this is mainly because of the amino (NH in aldehyde radical (CHO) in dialdehyde starch and collagen protein
2) having there is crosslinking reaction, the crosslinked network structure of a plurality of protein moleculars of formation is strengthened the reactive force between molecular chain, shows as the rising of film toughness in macroscopic view.When content is lower, along with the increase of content of crosslinking agent, dot density improves very fast, shows as tensile strength and rises.But due to the amino (NH in collagen protein
2) limited amount, therefore content of crosslinking agent to a certain extent after, it is saturated that crosslinking reaction is tending towards, continue to improve content, film toughness changes little, continuing to add residual aldehyde can affect the performance of film on the contrary, and when dialdehyde starch concentration reaches 0.20%, it is best that the tensile strength of collagen film and elongation at break all reach.
Compared with prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the present invention finds, forulic acid plays crosslinked effect to collagen film, can improve mechanical property and the barrier of film.In collagen concentration, be 10%, glycerol concentration is 2.83%, sodium alginate concentration is 0.60%, dialdehyde starch 0.41%, add under the condition of 0.28% forulic acid, the tensile strength of institute's film forming is 2.03MPa, elongation at break is 118.73%, water vapour permeability 0.25mL hm; Under same condition, do not add forulic acid, the tensile strength of institute's film forming is 1.87MPa, elongation at break is 112.58%; Water vapour permeability 0.28mL (hm); Forulic acid can be reacted and make collagen cross-linking with Methionin in collagen protein, halfcystine, tyrosine etc., adds water vapor, oxygen and carbonic acid gas transmitance that microdose of ferulic acid can improve the mechanical property of film and reduce film in film-forming soln.
(2) the present invention finds, forulic acid is added in collagen film and also given film with anti-microbial property as a kind of broad spectrum, natural antibacterial agent.It is 17-22mm to the antibacterial circle diameter of Gram-negative bacteria (intestinal bacteria) and Gram-positive (staphylococcus) that Oxford agar diffusion method records gained film, shows very strong bacteriostasis.
(3) the present invention finds, made edibility forulic acid-collagen protein antibacterial film not only has good packaging character, and there is very strong antibacterial ability, gained film liquid is sprayed to meat product as sausage surface, make its surface form a skim, thereby changed surface gas environment, effectively prevent juice loss, can maintain normal quality, taste, nutritive ingredient and outward appearance, and can suppress microorganism growth, to reach anti-corrosive fresh-keeping object, the sausage shelf-lives that found that interpolation edibility chitosan-collagen protein antibacterial film is compared with blank group sausage, can effectively completely cut off the route of entry of microorganism, delayed the chemical transformation of food ingredient, by the shelf life extension of sausage 8.5 days.
(4) compare with traditional packing film, collagen film has organic and inorganic component, the feature that biological material combines, other green substance are carried out to high added value Resource analysis: " turning waste into wealth ", be converted into the environmentally friendly packing material of excellent property, get back to directly or indirectly in material cycle, increased the amount of material cycle, do not cause environmental pollution.From the angle of material cycle, go to consider and the film that designs a package, for the research of the high added value of agricultural byproducts provides a thinking.
Accompanying drawing explanation
Fig. 1 is the variation of embodiment 1 product duration of storage total plate count.
Fig. 2 is the variation of embodiment 1 product duration of storage TVB-N value.
Fig. 3 is the variation of embodiment 1 product duration of storage pH value.
Fig. 4 is the variation of embodiment 1 product duration of storage sensory evaluation scores.
Embodiment
For understanding better the present invention; below in conjunction with embodiment, the present invention is described further; contriver is to by furtheing investigate and testing; there have been many successful embodiment; enumerate four specific embodiments below, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1:
Collagen protein is added to the water, in thermal treatment temp, it is stirring and dissolving under 60 ℃～70 ℃ conditions, add successively glycerine, dialdehyde starch, sodium alginate and forulic acid, in the mass concentration in solution, collagen concentration is 10%, forulic acid is 0.28%, and glycerine is 2.83%, and dialdehyde starch is 0.41%; Sodium alginate 0.6%.Under 60 ℃ of conditions, thermal treatment is 25 minutes, be placed in to stir defoamer and slough bubble, then on poly (methyl methacrylate) plate curtain coating, liquid cooling to be filmed is but placed in the baking oven of 60 ℃ and toasts 5 hours, cooling under normal temperature, then takes off film, makes forulic acid-collagen protein antibacterial film.The thickness of institute's film forming is 0.21mm.
The evaluation group that sets up 5 people, under noiseless environment, the film organoleptic detection situation becoming is as shown in table 1, and institute's film forming transparency, glossiness, surface flatness and smell situation are well, take off film easy.As shown in table 2, with reference to the compound edible film of the pumpkin-soybean protein isolates such as Xiao (ZhongKai Agriculture Engineering Academy journal, 25 3 phases of volume) moisture content that the method in records film is 84.7%, water-intake rate is 2.3%, the water droplet seepage time be 227.27min mm, water vapour permeability be 0.25g (hm).With reference to GB13022-91, the tensile strength that records film is 2.03MPa, and elongation at break is 118.73%.Adopting Oxford agar diffusion method to record intestinal bacteria and staphylococcic inhibition zone is the diameter 8mm of 20mm(Oxford cup).Above data show because forulic acid can be reacted and make collagen cross-linking with Methionin in collagen protein, halfcystine, tyrosine etc., in film-forming soln, add water vapor, oxygen and carbonic acid gas transmitance that microdose of ferulic acid can improve the mechanical property of film and reduce film, the plasticity and the dialdehyde starch that add glycerine can play crosslinking reaction with amino and the imino-of collagen protein, be prepared into there is transparent height, good barrier property, physical strength be higher, and has the edible food packaging film of anti-microbial property.Compared with prior art, another advantage of the present invention is that the material of gained film all derives from natural product, really has edibility; And raw material is easy to get, low price, simple to operate, there is very strong practical significance and feasibility.
The organoleptic quality of table 1 collagen film
The performance characterization of table 2 collagen film
With sterile brush, the sausage newly breaking a seal is divided into 3 groups at random, is labeled as respectively A, B and C.Wherein, A is control group, does not do any Preservation Treatment; B group adopts the collagen protein processing of filming; C group adopts the antibacterial film processing of filming.The sausages such as 3 groups of samples drain to be coated with and with PE preservative film, are packed after liquid, at room temperature place, and regularly getting a certain amount of sample carries out index of fish freshness mensuration.According to national standard SB/T10003-92 test, sausage one-level index of fish freshness is ㏒ (total plate count)≤4, and secondary index of fish freshness is 4 < ㏒ (total plate count)≤6, rotten Rou Wei ㏒ (total plate count) > 6; Sausage one-level index of fish freshness is TVB-N value≤15mg/100g, and secondary index of fish freshness is 15mg/100g < TVB-N value≤20mg/100g, and rotten meat is TVB-N value > 20mg/100g; Fresh sausage PH is 5.8-6.2, and inferior bright sausage PH is 6.3-6.6, and rotten meat is more than 6.7.
1. the variation of total plate count in preservation process
Pork putrid and deteriorated is the effect due to microorganism to a great extent, wherein, obvious with the effect of bacterium.The reproduction speed of bacterium is very fast, can along the reticular tissue of pork, blood vessel around or the gap of bone and muscle spread to and organize deep, therefore along with the variation of storage conditions and the development of metamorphic process, bacterium is invaded to deep gradually by the surface of meat, finally makes monoblock meat rotten.Meanwhile, the kind of bacterium also changes, and presents flora Alternate Phenomenon.And sausage is to take a kind of meat product that pork is raw material, therefore by measuring total plate count, can judge to a great extent the freshness of sausage.The total plate count that A, B in this experiment, C are tri-groups changes as shown in Figure 1.
From the data of Fig. 1, can find out: along with the prolongation of storage number of days, the total plate count of each group all in obvious increase, and film group and the total plate count of antibiotic group two groups gather way and are all starkly lower than control group.Wherein, the total plate count of control group increases the fastest, by the 11st day, reaches 9.78 * 10
5cFU/g, approaches the upper limit of secondary freshness, and within the 12nd day, total plate count reaches 1.2 * 10
6cFU/g, surpasses secondary index of fish freshness, illustrates that control group sausage is rotten at the 12nd day; And film group and the total plate count of antibiotic group are respectively at the 15th day and the 20th genius over secondary freshness.
The group of filming is the surface that collagen film covers sausage than the shelf life extension of the control group reason of 3 days, can effectively stop sausage to contact with air, thereby suppress aerobic growth.Therefore, group and the total plate count of antibiotic group two groups of filming early stage gap less, and along with the prolongation of time, the group of filming is because the antimicrobial factors in forulic acid-collagen protein antibacterial film discharges gradually in antibiotic group with the gap increase of antibiotic group, thereby can on sausage, bring into play anti-microbial activity, thereby slowed down the growth of sausage surface bacteria sum, make sausage shelf life extension 8 days.
2. the variation of TVB-N value in preservation process
Total volatile basic nitrogen (TVB-N) is meat decomposing protein produces under microbial process ammonia and rudimentary amine, amine substance is combined with the organic acid producing in decay process, having formed alkaline nitrogenous substances is deposited in meat, therefore its content is the very important index of reflection livestock and poultry meat, is also in national standard, to judge the important indicator of fresh meat standard.
As shown in Figure 2, the increase in time within storage period of the TVB-N value of sausage is in rising trend, and after 15 days, the TVB-N value of control group is 20.1mg/100g, just above the secondary index of fish freshness of sausage.In the group of filming, the TVB-N value of sausage reached 19.7mg/100g in the time of the 18th day, approached the upper limit of secondary freshness, and the 19th day is 20.8mg/100g, surpassed the value of regulation.Compare with control group, the shelf life extension of sausage 4 days.In antibiotic group, the TVB-N value of sausage reached 19.8mg/100g in the time of the 24th day, approached the upper limit of secondary freshness, and the 25th day is 20.3mg/100g, surpassed the value of regulation.Compare with control group, the shelf life extension of sausage 10 days.
When bacterium amount reproduction, TVB-N value can rapid growth, and now the total plate count of control group has exceeded standard, this may be because the corruption of vacuum-packed sausage to a great extent because lactobacter growth breeding produces lactic acid and volatile sulfur compounds causes
[58], the protein decomposition enzyme system of milk-acid bacteria a little less than, so TVB-N value lift velocity is less.
Coated by collagen sausage by the shelf life extension of sausage 4 days; reason is that collagen film forms the protective layer of even compact on sausage surface; have good barrier property, the growth and breeding of anti-bacteria preferably, has reduced the protein decomposition rate of sausage.And forulic acid-collagen protein antibacterial film has antibiotic and rot-resistant function, growth and breeding that can not only anti-bacteria, can also reduce the decomposition rate of protein, therefore experiment shows that antibacterial film can control the rate of growth of total volatile basic nitrogen to a certain extent, its fresh-keeping effect is better than collagen film, thereby extends the shelf-lives of sausage.
3. the variation of pH value in preservation process
The pH value of fresh pork is 7.2, the after death supply due to oxygen in blood circulation and body stops, glycogen generates pyruvic acid with glycolytic cycle declines human body pH value at flesh body accumulation, arrive after lower-most point, bacterium and enzyme decomposing protein produce alkaline matter, and pH value progressively rises again, so the degree of spoilage that the pH value of measuring meat sample also can indirect reaction sausage, pH value is higher, and degree of spoilage is larger.
Fig. 3 is the PH changing trend diagram of three groups of different treatment sausages, as can be seen from the figure, in general trend, film group and the PH rising amplitude of antibiotic group lower than control group, wherein film group and antibiotic group differ over time less, but data can be found out in figure, first the PH of control group reached 6.7 in the time of the 13rd day, and film group and the pH value of antibiotic group are respectively the 18th, 20 talentes reach 6.7, and the PH rangeability of control group is always maximum, in change procedure, higher than filming, organize and antibiotic group always, can illustrate that thus the group of filming is suppressed with the bacterial growth of antibiotic group of sausage, thereby protein decomposition rate slows down, make degree of spoilage lower than control group.In whole storage, although the pH value of antibiotic group is more or less the same with the group of filming, but from rangeability, the variation of antibiotic group is than the little of group of filming generally, and reach 6.7 the 20th talent, than the group of filming, extended 2 days, illustrated under the bacteriostatic action of forulic acid, the shelf life extension of sausage.
4. the variation of sensory evaluation scores in preservation process
By sense organ personnel, outward appearance, color and luster, smell, hardness, five Oranoleptic indicators of elasticity are carried out to Comprehensive Assessment, the organoleptic feature of food is to affect the important factor that human consumer selects, although there is certain subjectivity in sensory evaluation scores, but can for human consumer, reflect fast the information of quality product, therefore when carrying out the evaluation of meat product freshness, sensory evaluation scores is a very important evaluation index.
According to the regulation of national standard SB/T10003-92, the sausage of high-quality should possess following organoleptic feature: casing is dry complete, and is close to meat stuffing, without mucus and mildew; Solid or flexible; Tangent plane matter is close solid, and meat stuffing is glossy, and muscle bois de rose is to rose, and fat is white or redly micro-; There is the intrinsic smell of sausage.According to sausage subjective appreciation standards of grading, the sausage of duration of storage is marked, 3 groups of sausages are shown in Fig. 4 in the sensory evaluation scores variation tendency of duration of storage.
In figure, data are known, and along with the increase of time, the gap of three groups of sausage sensory evaluation scores values increases gradually.According within 6 minutes of the standard code of intestines sensory evaluation scores, showing below sample edible not, three groups of sausages respectively in the time of the 12nd, 16,20 days sensory evaluation scores approach 6, now sausage organoleptic feature presents the moistening and stickness of casing, easily separated with meat stuffing and easily tear, surface mildew is serious, after smearing, still has vestige; Tangent plane is uneven, and crack is obvious, and central part has ruckbildung; Meat stuffing is matt, and muscle look gloomy, and it is yellow that fat is; Rancidification taste is obvious, or has other peculiar smell.Therefore the group of filming by sausage shelf life extension 4 days, and antibiotic group by shelf life extension 8 days.The result reflecting due to sensory evaluation scores is the external manifestation of total plate count, TVB-N value and the PH variation of sausage, so the variation tendency of the variation tendency of its score value and Fig. 1, Fig. 2 and Fig. 3 has good consistence.
By the total plate count of three groups of sausages, TVB-N value, PH and sensory evaluation are measured, in line with take sensory evaluation scores as basic principle, and contrast the index of fish freshness of the sausage of three groups of different treatment, the antibacterial film that has added forulic acid can suppress pathogenic bacteria and the multiple breedings that cause the microorganism of food spoilage such as pneumobacillus, enterobacteria, intestinal bacteria due to forulic acid, effectively controlled the growth of total plate count, extend the shelf-lives 8.5 days of sausage, and collagen film is only by shelf life extension 4 days.The shelf-lives of three groups of sausages is as shown in table 3:
Table 3 sausage shelf-lives
Tab.2The?shelf-life?of?sausage
Embodiment 2:
A kind of preparation method of forulic acid-collagen protein antibacterial film: collagen protein is added to the water, in thermal treatment temp, it is stirring and dissolving under 70 ℃ of conditions, add successively glycerine, dialdehyde starch, sodium alginate and forulic acid, in the mass concentration in solution, collagen concentration is 6%, forulic acid is 0.30%, and glycerine is 2.40%, and dialdehyde starch is 0.60%; Sodium alginate 0.40%.Under 70 ℃ of conditions, thermal treatment is 20 minutes, be placed in to stir defoamer and slough bubble 18min, then on poly (methyl methacrylate) plate curtain coating, liquid cooling to be filmed is but placed in the baking oven of 60 ℃ and toasts 5 hours, cooling under normal temperature, then take off film, make forulic acid-collagen protein antibacterial film.The thickness of institute's film forming is 0.21mm.The film organoleptic detection situation becoming is as shown in table 1.With reference to the compound edible film of the pumpkin-soybean protein isolates such as Xiao (ZhongKai Agriculture Engineering Academy journal, 25 3 phases of volume) moisture content that the method in records film is 90.2%, water-intake rate is 3.4%, the water droplet seepage time be 160min mm, water vapour permeability be 18g (hm), with reference to GB13022-91, the tensile strength that records film is 1.41MPa, and elongation at break is 115.24%.Adopting Oxford agar diffusion method to record intestinal bacteria and staphylococcic inhibition zone is the diameter 8mm of 20mm(Oxford cup)
Embodiment 3:
A kind of preparation method of forulic acid-collagen protein antibacterial film: collagen protein is added to the water, in thermal treatment temp, it is stirring and dissolving under 65 ℃ of conditions, add successively glycerine, dialdehyde starch, sodium alginate and forulic acid, in the mass concentration in solution, collagen concentration is 14%, forulic acid is 0.14%, and glycerine is 2.80%, and dialdehyde starch is 0.28%; Sodium alginate 1.68%.Under 65 ℃ of conditions, thermal treatment is 30 minutes, be placed in to stir defoamer and slough bubble 19min, then on poly (methyl methacrylate) plate curtain coating, liquid cooling to be filmed is but placed in the baking oven of 60 ℃ and toasts 4 hours, cooling under normal temperature, then take off film, make forulic acid-collagen protein antibacterial film.The thickness of institute's film forming is 0.21mm.The film organoleptic detection situation becoming is as shown in table 1.With reference to the compound edible film of the pumpkin-soybean protein isolates such as Xiao (ZhongKai Agriculture Engineering Academy journal, 25 3 phases of volume) moisture content that the method in records film is 88.24%, water-intake rate is 2.8%, the water droplet seepage time be 210.57min mm, water vapour permeability be 24g (hm), with reference to GB13022-91, the tensile strength that records film is 1.95MPa, and elongation at break is 119.73%.Adopting Oxford agar diffusion method to record intestinal bacteria and staphylococcic inhibition zone is the diameter 8mm of 15mm(Oxford cup)
Embodiment 4:
A kind of preparation method of forulic acid-collagen protein antibacterial film: collagen protein is added to the water, in thermal treatment temp, it is stirring and dissolving under 60 ℃ of conditions, add successively glycerine, dialdehyde starch, sodium alginate and forulic acid, in the mass concentration in solution, collagen concentration is 8%, forulic acid is 0.24%, and glycerine is 2.40%, and dialdehyde starch is 0.48%; Sodium alginate 0.48%.Under 65 ℃ of conditions, thermal treatment is 25 minutes, be placed in to stir defoamer and slough bubble 17min, then on poly (methyl methacrylate) plate curtain coating, liquid cooling to be filmed is but placed in the baking oven of 60 ℃ and toasts 6 hours, cooling under normal temperature, then take off film, make forulic acid-collagen protein antibacterial film.The thickness of institute's film forming is 0.21mm.The film organoleptic detection situation becoming is as shown in table 1.With reference to the compound edible film of the pumpkin-soybean protein isolates such as Xiao (ZhongKai Agriculture Engineering Academy journal, 25 3 phases of volume) moisture content that the method in records film is 82.1%, water-intake rate is 1.98%, the water droplet seepage time be 237.47min mm, water vapour permeability be 22g (hm), with reference to GB13022-91, the tensile strength that records film is 2.33MPa, and elongation at break is 118.73%.Adopting Oxford agar diffusion method to record intestinal bacteria and staphylococcic inhibition zone is the diameter 8mm of 18mm(Oxford cup).
As can be seen from the above embodiments, forulic acid can be reacted and make collagen cross-linking with Methionin in collagen protein, halfcystine, tyrosine etc., in film-forming soln, add water vapor, oxygen and carbonic acid gas transmitance that microdose of ferulic acid can improve the mechanical property of film and reduce film, the plasticity and the dialdehyde starch that add glycerine can play crosslinking reaction with amino and the imino-of collagen protein, are prepared into have transparent height, good barrier property, certain physical strength, have the edible food packaging film of anti-microbial property.Also give film with anti-microbial property, it is 17-22mm to the antibacterial circle diameter of Gram-negative bacteria (intestinal bacteria) and Gram-positive (staphylococcus) that Oxford agar diffusion method records gained film, show very strong bacteriostasis, by this film be coated on sausage fresh-keeping in, can be by sausage shelf life extension 8.5 days.In addition, compare with traditional packing film, collagen film has organic and inorganic component, the feature that biological material combines, other green substance are carried out to high added value Resource analysis: " turning waste into wealth ", be converted into the environmentally friendly packing material of excellent property, get back to directly or indirectly in material cycle, increase the amount of material cycle, do not caused environmental pollution.From the angle of material cycle, go to consider and the film that designs a package, for the research of the high added value of agricultural byproducts provides a thinking.
Claims (9)
1. the preparation method of forulic acid-collagen protein antibacterial film, it is characterized in that: collagen protein is added to the water, in thermal treatment temp, it is stirring and dissolving under 60 ℃～70 ℃ conditions, add successively glycerine, dialdehyde starch, sodium alginate and forulic acid, thermal treatment 20-30 minute under 60 ℃～70 ℃ conditions, is placed in stirring defoamer and sloughs bubble, curtain coating on poly (methyl methacrylate) plate again, liquid cooling to be filmed is post-drying but, cooling under normal temperature, take off film, makes forulic acid-collagen protein antibacterial film; In the mass concentration in solution, collagen concentration is 6-14%, and forulic acid is 0.06-0.70%, and glycerine is 1.20-5.60%, and dialdehyde starch is 0.12-1.4%, sodium alginate 0.24-1.68%.
2. the preparation method of forulic acid-collagen protein antibacterial film according to claim 1, is characterized in that: described oven dry is to be placed in the baking oven of 60 ℃ to toast 4-6h.
3. the preparation method of A Wei acid ?collagen protein antibacterial film according to claim 1, is characterized in that: in the mass concentration in solution, described collagen concentration is 8 ?12%.
4. the preparation method of A Wei acid ?collagen protein antibacterial film according to claim 1, is characterized in that: in the mass concentration in solution, described glycerol concentration is 1.60 ?3.60%.
5. the preparation method of A Wei acid ?collagen protein antibacterial film according to claim 1, is characterized in that: in the mass concentration in solution, described sodium alginate concentration is 0.40 ?0.84%.
6. the preparation method of A Wei acid ?collagen protein antibacterial film according to claim 1, is characterized in that: in the mass concentration in solution, described dialdehyde starch concentration is 0.40 ?0.60%.
7. the preparation method of A Wei acid ?collagen protein antibacterial film according to claim 1, is characterized in that: in the mass concentration in solution, described forulic acid concentration is 0.16 ?0.36%.
8. forulic acid-collagen protein antibacterial film, is characterized in that it is made by preparation method described in claim 1-7 any one.
9. the application of forulic acid-collagen protein antibacterial film on food preservation described in claim 8.
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| CN105254928A (en) * | 2015-11-26 | 2016-01-20 | 广西大学 | Preparing method for ferulic acid-chitosan active packaging film |
| CN107183150A (en) * | 2017-06-13 | 2017-09-22 | 扬州大学 | A kind of preservation method of belt leather Xiangsha dasheen |
| CN107722644A (en) * | 2017-09-30 | 2018-02-23 | 铜陵家宴生态农业发展有限公司 | A kind of freeze-thawing resistant forulic acid is modified the preparation method of banana tegument extract composite membrane |
| CN108522633A (en) * | 2018-03-27 | 2018-09-14 | 浙江工商大学 | A kind of multiple preserving antistaling agent composition formula and application containing ferulic acid butyl ester |
| CN110240808A (en) * | 2019-06-24 | 2019-09-17 | 东北农业大学 | A kind of inoxidizability soybean protein laminated film and preparation method thereof |
| CN111012771A (en) * | 2020-01-08 | 2020-04-17 | 辽宁大学 | Application of ferulic acid in preparation of medicine for inhibiting chromium-induced lung inflammatory injury |
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| CN112940315B (en) * | 2021-02-05 | 2023-03-14 | 天津科技大学 | Preparation method and application of nano collagen membrane |
| CN114773689A (en) * | 2021-12-30 | 2022-07-22 | 中国农业大学 | Ferulic acid-arabinoxylan copolymer antibacterial film, preparation method and application |
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